CN101313939A - Corydalis saxicola total alkaloid, preparation method and uses thereof - Google Patents

Corydalis saxicola total alkaloid, preparation method and uses thereof Download PDF

Info

Publication number
CN101313939A
CN101313939A CNA2007100996879A CN200710099687A CN101313939A CN 101313939 A CN101313939 A CN 101313939A CN A2007100996879 A CNA2007100996879 A CN A2007100996879A CN 200710099687 A CN200710099687 A CN 200710099687A CN 101313939 A CN101313939 A CN 101313939A
Authority
CN
China
Prior art keywords
rhizoma coptidis
alkaloid
salt
rock
add
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CNA2007100996879A
Other languages
Chinese (zh)
Inventor
王锦刚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Kexin Bicheng Medicine Technology Development Co Ltd
Original Assignee
Beijing Kexin Bicheng Medicine Technology Development Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing Kexin Bicheng Medicine Technology Development Co Ltd filed Critical Beijing Kexin Bicheng Medicine Technology Development Co Ltd
Priority to CNA2007100996879A priority Critical patent/CN101313939A/en
Publication of CN101313939A publication Critical patent/CN101313939A/en
Pending legal-status Critical Current

Links

Images

Abstract

The invention provides a method for extracting and preparing corydalis saxicola bunting total alkaloid, which is applied to the extraction of the corydalis saxicola bunting total alkaloid by taking corydalis saxicola bunting plants as raw materials. The method has the advantages of effectively combining unit operations of acid water extraction, salting out and active carbon decoloring and degreasing, etc.; moreover, products obtained by the method have the advantages of stable and uniform color and luster, high content of effective components and good melting property, and corydalis saxicola bunting injections prepared by the materials obtained by the method have the advantages of good clarity, high extraction yield of the corydalis saxicola bunting total alkaloid and low manufacturing cost.

Description

Total alkaloids of meadowrueleaf corydalis root and preparation method thereof and purposes
Technical field
The invention belongs to medical technical field, relate to a kind of total alkaloids of meadowrueleaf corydalis root, also relate to the preparation method and the purposes in the preparation medicine thereof of this meadowrueleaf corydalis root extract.
Background technology
Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) is bloodroot Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) (Corydalis thalictrifolia Franch., Radix CorydalisThalinctrifoliae), and the different name rock recklessly.Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae), perennial book on Chinese herbal medicine, root turbination, meat, stem is single or grow thickly high 15-20 centimetre, the base of leaf base is given birth to, and the blade keratin is with the shape compound leaf, vanelets mostly is 3 drastic cracks or 3 shallow splitting, and last sliver tip circle is blunt, and give birth on the raceme top, capsule is linear, and is membranous, yellow, 2 lobes split when ripe, and seed is tiny, grows in Shi Yanshang.Mountain areas such as distribution and Guizhou.Have functions such as heat-clearing and toxic substances removing, dampness removing, analgesic hemostatic.Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) mainly is used as medicine with root.Have effects for removing toxic heat, be applicable to acute, chronic hepatitis dampness-heat in the liver and gallbladder disease person.
It with the Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) treatment that Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) injection that raw material is made once was used for hepatopathys such as hepatitis, hepatic fibrosis.The Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) injection from calendar year 2001 December be put into national standard tentative 2 years, what be put into simultaneously also has meadowrueleaf corydalis root extract.In the standard of extract, be assay with the total alkaloids of meadowrueleaf corydalis root of measuring in the meadowrueleaf corydalis root extract wherein, the content of total alkaloids of meadowrueleaf corydalis root is not less than 3.4% in the exsiccant extract.
The main problem that exists of legal total alkaloids of meadowrueleaf corydalis root extracting method (seeing National Drug Administration's " national standard for traditional Chinese medicines compilation " internal medicine liver and gall fascicle in 2002, the 325-328 page or leaf) be pilot process loaded down with trivial details and cause that later stage quality formulation products (injection) quality is wayward, stability and clarity be relatively poor.In addition, disclosed total alkaloids of meadowrueleaf corydalis root also has disclosed several method among the Chinese patent CN1185231C in the prior art, as alcohol extraction follow the example of, acid extraction method, organic solvent extraction method, but all need after obtaining crude extract, wait purification, and then improve total alkaloid contents in the crude extract with resin method, the amine salt sedimentation method, Amberlyst process.This makes that whole leaching process is more loaded down with trivial details, and because later stage use resin method etc. need a large amount of organic solvents, has promptly increased cost, makes the later stage have poisonous organic solvent residue again in preparation.
Therefore, it is simple to press for a kind of extraction process, guarantees again to meet official quality standands, and can not increase later stage preparation intractability, lower-cost corydalis saxicola total alkaloid extract and preparation method thereof.
Summary of the invention
The purpose of this invention is to provide extract of a kind of new total alkaloids of meadowrueleaf corydalis root and preparation method thereof.
In second aspect, the invention provides the various preparations that make by aforementioned total alkaloids of meadowrueleaf corydalis root.
In the third aspect, the invention provides the purposes in preparation treatment hepatitis disease by aforesaid corydalis saxicola total extract and preparation thereof.
In fourth aspect, the invention provides the compositions of forming by aforesaid total alkaloids of meadowrueleaf corydalis root and medically effective treating hepatitis medicine.
Aspect the 5th, the invention provides the preparation of making in pharmaceutically acceptable carrier by above-mentioned composition.
Aspect the 6th, the invention provides the purposes of this above-mentioned preparation in the medicine of preparation treatment hepatitis and relevant disease thereof.
Aspect the 7th, the invention provides the test kit of forming by aforesaid total alkaloids of meadowrueleaf corydalis root and medically effective treating hepatitis medicine.
In eight aspect, the invention provides the purposes of this mentioned reagent box in the medicine for the treatment of hepatitis and relevant disease thereof as treatment.
Corydalis saxicola total alkaloid extract provided by the invention is made by following steps:
1 to get rock Rhizoma Coptidis plant herb an amount of, is crushed to coarse powder, adds 4~15 times of amount aqueous sulfuric acid (0.1~1%) soak at room temperature and extracted 24 hours, filters.
2 get the Sal (NaCl) of extracting solution adding 10~20%, saltout under continuous stirring, place 8 ~ 12 hours, filter and collect rock Rhizoma Coptidis alkaloid sulfate precipitation.
3 are dissolved in alkaloid precipitation in 20 times the ethanol, add an amount of active carbon, and reflux was decoloured in 30 minutes, filtered, and filtrate concentrates and reclaims ethanol, and the concentrate drying product are rock Rhizoma Coptidis alkaloid.
4 are dissolved in above gained rock Rhizoma Coptidis alkaloid in 5~10% an amount of aqueous hydrochloric acid solutions, filter, and the filtrate decompress(ion) is concentrated into dried, promptly gets rock Rhizoma Coptidis alkaloid salt hydrochlorate.
Can make appropriate formulation with pharmaceutically acceptable carrier combinations by the above-mentioned corydalis saxicola total alkaloid extract that obtains uses.It can oral administration or through parenterai administration.For oral administration, can use known form of medication, for example tablet, capsule, sugar coated tablet etc.
Equally compatibly can be liquid or semi-liquid form, oral liquid for example, this medicament exists with solution or form of suspension in the case.Operable solution or suspending agent are water, aqueous medium or pharmaceutically acceptable oils (vegetable oil or mineral oil).Contain above-mentioned corydalis saxicola total alkaloid extract and also can be made into sustained-release preparation, this type of preparation can the mode with slow controlled release discharge medicine in vivo in the long time.
In addition, can also make rectum (for example passing through suppository) according to corydalis saxicola total alkaloid extract of the present invention, inhalation (aerosol that specific concentrations and particle size distribution are arranged by suction), percutaneous dosing (patch by containing activating agent, liniment solution, gel etc.), mucosal (through port and Nasal Mucosa Absorption medicine, or enter nasal cavity etc. by injection), by implant form administration (the passive infiltration of medicine or by the controlled release of Micropump), by administration in vein, intramuscular injection or subcutaneous injection and the brain ventricle.
About parenterai administration, preferably with injection and/or freeze-dried powder form administration.
According to the present invention, corydalis saxicola total alkaloid extract can be used for the treatment of with the form of its free alkali and addition salts, and preferred salt is the hydrochlorate and the corydalis saxicola total alkaloid extract sulfate of corydalis saxicola total alkaloid extract.In addition, also may use the salt of acceptable acid on other pharmacology, for example phosphoric acid, hydrobromic acid, acetic acid, methanesulfonic acid, citric acid, tartaric acid, fumaric acid etc.
The pharmaceutical preparation that is used for the corydalis saxicola total alkaloid extract administration according to the present invention can comprise one or more following additives: a antioxidant, synergist, stabilizing agent, b antiseptic, c correctives, the d pigment, the e solvent, solubilizing agent, f surfactant, g influences the reagent of viscosity and denseness, gel former, h absorption enhancer, I absorbent, wetting agent, fluidizer; The j slow releasing agent.These additives are not limited thereto, for any suitable physiologically acceptable carrier well known to those of ordinary skill in the art all can adopt.
The ratio that comprises corydalis saxicola total alkaloid extract in the preparation is 0.1-99wt%, and active substance calculates with free corydalis saxicola total alkaloid extract in all cases.Can further comprise additive according to the pharmaceutical preparation that contains corydalis saxicola total alkaloid extract used in the present invention, as non-active ingredient, excipient, vehicle and/or stabilizing agent, its amount is known by the routine techniques means by those of ordinary skills.Prepared corydalis saxicola total alkaloid extract preparation dosage every day is for deciding according to the individuality for the treatment of, preferred consumption is the optimum consumption that does not produce significant side effects and can reach the effect of being wanted, and those of ordinary skills can well do suitable adjustment according to the requirement of individuality fully.
Total alkaloids of meadowrueleaf corydalis root provided by the present invention is preferred for hepatitis and the related indication treatment that various viruses cause.
Employed term " hepatitis " is meant anxious, the dirty inflammation of chronic hepatitis that is caused by various viruses (as hepatitis A, second sexual type hepatitis, hepatitis C, hepatitis D, hepatitis E) among the application, and by these viral complication that causes liver's inflammation.
The compositions that corydalis saxicola total alkaloid extract that the application provides and medically effective treating hepatitis medicine are formed, comprise in the medicine of the corydalis saxicola total alkaloid extract addressed previously and following treatment hepatitis one or more: (a) suppress virus protein in conjunction with and/or the chemical compound of infection cell, comprise antibody (as monoclonal antibody) and glucamine polysaccharide (as the sulfate or the suramin of heparin) at virus itself; (b) suppress virus discharges and suppress viral function gene expression from virus coat chemical compound, comprise IRES inhibitor, protease inhibitor (as serine protease); (c) chemical compound of interfere with or compromise cellular replication comprises trophicardyl list monophosphate dehydrogenase inhibitor (as virazole, mycophenolic acid and VX497) and glycoprotein reaction suppressor, as DNJ and mortifier thereof; (d) chemical compound (as extrasin alpha and α or interferon-) of change immunologic function; (e) play the chemical compound (as joining this pair fat, phosphocholine, silibinin, taurine, glycyrrhizic acid diamidogen, tiopronin matrine, inositol, extension base of a fruit element, orazamide etc.) that improves hepatitis symptom.
These medically effectively treating hepatitis medicines can with total alkaloids of meadowrueleaf corydalis root of the present invention simultaneously, separate, use successively.If non-while administration, the other medicines of treatment hepatitis should not reduce the synergistic therapeutic action between each component.
The preferred interferon-alpha of using can also be used other interferon certainly.
Above-mentioned composition can also contain a kind of pharmaceutically acceptable excipient arbitrarily.
The present invention ground total alkaloids of meadowrueleaf corydalis root is compared with extraction ground total alkaloids of meadowrueleaf corydalis root in the prior art, has therapeutic effect better, has curative effect better at aspects such as reducing hepatitis B patient ground jaundice,
Compositions of the present invention is preferred for hepatitis and the related indication treatment that various viruses cause.
On the other hand, the present invention also provides a kind of test kit, contain total alkaloids of meadowrueleaf corydalis root and in the following compounds one or more in any claim in front in its basis: (a) suppress virus protein in conjunction with and/or the chemical compound of infection cell, comprise antibody and glucamine polysaccharide at virus itself; (b) suppress virus discharges and suppress viral function gene expression from virus coat chemical compound; (c) chemical compound of interfere with or compromise cellular replication; (d) chemical compound of change immunologic function; (e) play chemical compound and/or the plant extract that improves hepatitis symptom.
Also contain in this test kit and be used for the treatment of hepatitis and related indication operation instructions thereof.
Total alkaloids of meadowrueleaf corydalis root of the present invention and medically effective treating hepatitis medicine can load in mixture in same dosage form units.
Describe the present invention below in conjunction with embodiment, these embodiment myopia further specify the application's, and do not play any qualification effect.
Description of drawings
Accompanying drawing 1 is the extraction process flow chart of salt Rhizoma Coptidis total alkaloids
Embodiment
The extraction of salt Rhizoma Coptidis total alkaloids
1) statutory standards with the GB record compare test
Be soluble in the character of sour water according to main effective ingredient alkaloid in the Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae), adopt orthogonal design to filter out the optimum process condition of Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) sulphuric acid water extraction, and with saltout, dissolve with ethanol takes off assorted and monotechnics efficient in operation combination such as activated carbon decolorizing, make and extract operation more rationally effectively, also with corresponding legal technology (National Drug Administration's " national standard for traditional Chinese medicines compilation " internal medicine liver and gall fascicle in 2002, the 325th~328 page) compare research, determine the feasibility and the superiority of new technology.
One, the assay of Corydalis Saxicolae
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With acetonitrile-water (containing 0.34% potassium dihydrogen phosphate and 0.1% dodecyl sodium sulfate) (32: 68) is mobile phase; The detection wavelength is 347nm.Number of theoretical plate calculates by the Corydalis Saxicolae peak should be not less than 8000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Corydalis Saxicolae reference substance, adds mobile phase and make the solution that every 1ml contains 0.13mg.
The preparation of need testing solution: precision takes by weighing this product 10mg (or suitable test specimen amount), adds the mutual-assistance dissolving of flowing, and is settled to 10ml, filters, and gets subsequent filtrate, promptly.
Algoscopy: precision is drawn reference substance solution and each 10ul of need testing solution respectively, injects chromatograph of liquid, measures, and both calculates to get.
Two, the comparative study of Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) Different Extraction Method and technological parameter
2.1 the foundation of assay and quality evaluating method: with reference to National Drug Administration's " national standard for traditional Chinese medicines compilation " internal medicine liver and gall fascicle in 2002, the 325th~328 page relevant technologies required to carry out.
2.2 former legal extraction process checking
Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) is ground into coarse powder, takes by weighing Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) coarse powder 500g and add 90% ethanol 4.5L, flooded 24 hours, hot reflux is extracted 4 times, each 1 hour.Merge extractive liquid,, decompression recycling ethanol also is concentrated into the clear paste that relative density is 0.92~1.02 (60 ℃), puts coldly, filters filtrate and is concentrated into the silk fabric cream that relative density is 1.16~1.20 (60 ℃).In silk fabric cream, add an amount of distilled water, use 10% hydrochloric acid solution, regulate pH value to 2~3, stir fully, filter, wash 4~5 times, merge acid liquid, regulate pH value to 9~10 with sodium carbonate with 10% hydrochloric acid solution, separate out brown precipitation, filter filtering residue chloroform extraction 5~6 times, combined chloroform liquid, add anhydrous sodium sulfate dehydration, filter, reclaim chloroform and do near, add a small amount of ethanol again, decompression and solvent recovery, drying, promptly get meadowrueleaf corydalis root extract, repeat 5 times, on average obtain meadowrueleaf corydalis root extract 8.8g.
The former legal extraction process demonstration test of table 1.
Find former legal extraction process having aspect many imperfections in the production implementation process in the proof procedure:
Extract the Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) powder with 90% alcohol dipping, hot reflux, gained clear paste chlorophyll and oiliness composition are too many, thereby cause very difficulty of follow-up filtration, and chlorophyll is difficult to separate thoroughly with the oiliness composition;
Owing to above reason, chlorophyll in the chloroform extract and oiliness component content are higher, cause the control of follow-up formulation products (injection) difficult quality, and heavy lightness of solution and stability are undesirable.
2.3 orthogonal test sulphuric acid water retting extraction process (flow process is referring to Figure of description 1)
2.3.1 the preliminary trial test of the relation of concentration sulphuric acid and extraction ratio: get 4 parts in 50g Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) powder respectively, reuse 0.1%, 0.5%, 1.0%, 1.5% aqueous sulfuric acid 1000ml dipping extracted 48 hours, filter, measure the content of Corydalis Saxicolae in the extracting solution, calculate extraction ratio (seeing Table 2.), test shows 0.5% sulphuric acid extraction rate height.
The relation of table 2. variable concentrations sulphuric acid and extraction ratio
Content is with 0.8% note in the medical material
2.3.2 Orthogonal Experiment and Design: according to the result of preliminary trial test, draft 3 kinds of factors, every kind of factor is selected 3 levels (table 3), by L9 (33) orthogonal designs (table 4) Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) is flooded and extracts experiment.
Table 3. factor level table
Figure A20071009968700111
2.3.3 extraction operational approach: take by weighing Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) powder 50g respectively, press factor and level that orthogonal test table 3 is selected, add 0.5% aqueous sulfuric acid dipping and extract, filtrate is for test.
2.3.4 determining of sulphuric acid water retting extraction process: just test the gained result and carry out intuitive analysis and see Table 4.According to extreme difference value Rk as can be seen, each factor is successively decreased by C, A, B in proper order to the influence of Corydalis Saxicolae extracted amount in the Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae), and process conditions are A3B2C3 preferably.Extract Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) with this, the Corydalis Saxicolae extracted amount is 312.9mg/500g, only extracts 1 time with test 7 in the table 4 and compares, though extracted amount slightly increases, extracting solution increases by 1 times of amount, and the time also increases by 1 times of amount.Therefore, reduce cost, save the consideration of raw material and time from produce, the optimum process condition that the sulphuric acid water retting extracts should be A3B1C3, be about to the Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) pulverizing medicinal materials and become coarse powder, add 16 times of amount 0.5% aqueous sulfuric acid dippings and extracted 48 hours, extract 1 time, get final product.
Table 4.L9 (33) test arrangement and experimental result
Figure A20071009968700121
Improve extraction process and corresponding legal extraction process comparative test:
Get 40 kilograms of Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) coarse powder, mixing is divided into 4 equal portions, presses the extraction of improvement technology for optional two parts, extract by legal technology in addition, and with rock Rhizoma Coptidis alkali content, dissolubility, indexs such as solution clarity compare.
Table 5. improves extraction process and corresponding legal extraction process technology index compares
Figure A20071009968700122
Conclusion: according to rock Rhizoma Coptidis alkali content, dissolubility, solution clarity to two kinds of extraction processes are relatively improved technology and will obviously be better than legal technology, but also have evaded toxic reagent such as chloroform, have guaranteed that effectively no toxic reagent is residual in the terminal preparation.
The technology stability test
Get Corydalis thalictrifolia Franch. (Radix Corydalis Thalictrifoliae) coarse powder 10 at every turn and extract 5 batches of test productions continuously by improving the technology extraction process, to the rock Rhizoma Coptidis alkali content of extract, dissolubility, indexs such as solution clarity detect, and judge the stability of improving extraction process with this.
The test data sheet of table 6. technology stability
Extract the test sequence number Rock Rhizoma Coptidis alkali content Dissolubility The solution clarity Remarks
1 21.75 Water solublity is good Clarity is good
2 19.60 Water solublity is good Clarity is good
3 22.09 Water solublity is good Clarity is good
4 20.53 Water solublity is good Clarity is good
5 22.59 Water solublity is good Clarity is good
Conclusion: extract continuously to test and produce 5 batches of presentation of results, it is more stable reliable to improve the technology extraction process, extracts production operation smoothness smoothly.
Specific embodiment
Specific embodiment one
1, gets rock Rhizoma Coptidis plant herb 40Kg, be crushed to coarse powder, add 400Kg aqueous sulfuric acid (0.1~1%) soak at room temperature and extracted 24 hours, filter.
2, get extracting solution, under continuous stirring, add 60Kg Sal (NaCl), saltout, placed 10 hours, filter, collect and obtain rock Rhizoma Coptidis alkaloid sulfate precipitation 412g.
3, the alkaloid precipitation is dissolved in 1 liter of ethanol, adds the 50g active carbon, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrated and obtained rock Rhizoma Coptidis alkaloid dry product 301g.
4, above gained rock Rhizoma Coptidis alkaloid is dissolved in 2 liters 20% aqueous hydrochloric acid solution, filters, filtrate is concentrated into dried, obtains rock Rhizoma Coptidis alkaloid salt hydrochlorate 316g.
Specific embodiment two
1, gets rock Rhizoma Coptidis plant herb 80Kg, be crushed to coarse powder, add 800Kg aqueous sulfuric acid (0.1~1%) soak at room temperature and extracted 24 hours, filter.
2, get extracting solution, under continuous stirring, add 120Kg Sal (NaCl), saltout, placed 10 hours, filter, collect and obtain rock Rhizoma Coptidis alkaloid sulfate precipitation 833g.
3, the alkaloid precipitation is dissolved in 2 liters of ethanol, adds the 100g active carbon, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrated and obtained rock Rhizoma Coptidis alkaloid dry product 635g.
4, above gained rock Rhizoma Coptidis alkaloid is dissolved in 4 liters 20% aqueous hydrochloric acid solution, filters, the filtrate decompress(ion) is concentrated into dried, obtains rock Rhizoma Coptidis alkaloid salt hydrochlorate 641g.
Specific embodiment three
1, gets rock Rhizoma Coptidis plant herb 120Kg, be crushed to coarse powder, add 1200Kg aqueous sulfuric acid (0.1~1%) soak at room temperature and extracted 24 hours, filter.
2, get extracting solution, under continuous stirring, add 180Kg Sal (NaCl), saltout, placed 10 hours, filter, collect and obtain rock Rhizoma Coptidis alkaloid sulfate precipitation 1305g.
3, the alkaloid precipitation is dissolved in 3 liters of ethanol, adds the 150g active carbon, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrated and obtained rock Rhizoma Coptidis alkaloid dry product 910g.
4, above gained rock Rhizoma Coptidis alkaloid is dissolved in 6 liters 20% aqueous hydrochloric acid solution, filters, the filtrate decompress(ion) is concentrated into dried, obtains rock Rhizoma Coptidis alkaloid salt hydrochlorate 964g.
Conclusion: use above method all can be relatively and the method in the national standard more effectively extract the salt Rhizoma Coptidis total alkaloids.
The preparation of rock Rhizoma Coptidis total alkaloids
Tablet: mg/ sheet
Salt Rhizoma Coptidis total alkaloids extract 105
Lactose 100
Starch 25
Polyvidone 2
Magnesium stearate 2
234
Conclusion: salt Rhizoma Coptidis total alkaloids extract can well be pressed into tablet.
Some specific embodiments are described and illustrate in the present invention, and what one of ordinary skill in the art will appreciate that is various changes, variation, modification, replacement, removal or the interpolation that can carry out within the spirit and scope of the present invention test.Therefore, this means the present invention can define with following claim with these claim with wide as far as possible reasonable dismissal.

Claims (21)

1 one kinds of salt Rhizoma Coptidis total alkaloids extracts is characterized in that being made by the following steps extraction:
1) it is an amount of to get rock Rhizoma Coptidis plant herb, is crushed to coarse powder, adds 0.1~1% aqueous sulfuric acid, and soak at room temperature extracted 24-48 hour, filter,
2) get extracting solution and add NaCl, under continuous stirring, saltout, placed 8-12 hour, filter and collect rock Rhizoma Coptidis alkaloid sulfate precipitation,
3) the alkaloid precipitation is dissolved in the ethanol, adds an amount of active carbon, the reflux decolouring is filtered, and filtrate concentrates and reclaims ethanol, and the concentrate drying product are rock Rhizoma Coptidis alkaloid.
2 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 1 is characterized in that being made by the following steps extraction:
1) it is an amount of to get rock Rhizoma Coptidis plant herb, is crushed to coarse powder, adds 4~16 times of amount 0.1~1% aqueous sulfuric acids, and soak at room temperature extracted 24 hours, filter,
2) get extracting solution and add 10~20% NaCl, under continuous stirring, saltout, placed 8-12 hour, filter collection rock Rhizoma Coptidis alkaloid sulfate precipitation,
3) the alkaloid precipitation is dissolved in the ethanol of 20 times of weight, adds an amount of active carbon, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaims ethanol, and the concentrate drying product are rock Rhizoma Coptidis alkaloid.
3 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 1 is characterized in that being made by the following steps extraction:
1), get rock Rhizoma Coptidis plant herb, be crushed to coarse powder, add 10 times of amount 0.1~1% aqueous sulfuric acids, soak at room temperature extracted 24 hours, filter,
2), get extracting solution, under continuous stirring, add 1.5 times of weight NaCl, saltout, placed 10 hours, filter, collection obtains rock Rhizoma Coptidis alkaloid sulfate precipitation,
3), alkaloid precipitation is dissolved in 20 times of weight ethanol, add 1.25 times of weight active carbons, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrates and obtains rock Rhizoma Coptidis alkaloid dry product.
4 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 1 is characterized in that being made by the following steps extraction:
1), get rock Rhizoma Coptidis plant herb, be crushed to coarse powder, add 16 times of amount 0.1~1% aqueous sulfuric acids, soak at room temperature extracted 48 hours, filter,
2), get extracting solution, under continuous stirring, add 1.5 times of weight NaCl, saltout, placed 10 hours, filter, collection obtains rock Rhizoma Coptidis alkaloid sulfate precipitation,
3), alkaloid precipitation is dissolved in 20 times of weight ethanol, add 1.25 times of weight active carbons, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrates and obtains rock Rhizoma Coptidis alkaloid dry product.
The salt of any salt Rhizoma Coptidis total alkaloids extract of 5 claim 1-4 is characterized by the salt Rhizoma Coptidis total alkaloids is dissolved in the corresponding acid solution and filters, and the filtrate decompress(ion) is concentrated into dried, promptly gets the corresponding salt of rock Rhizoma Coptidis alkaloid.
The salt of 6 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 5, wherein acid can be selected from one or more in hydrobromic acid, acetic acid, methanesulfonic acid, citric acid, tartaric acid, phosphoric acid, the fumaric acid.
The salt of 7 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 5, wherein acid is hydrochloric acid.
The extracting method of 8 one kinds of salt Rhizoma Coptidis total alkaloids extracts is characterized in that:
1) it is an amount of to get rock Rhizoma Coptidis plant herb, is crushed to coarse powder, adds 0.1~1% aqueous sulfuric acid, and soak at room temperature extracted 24 hours, filter,
2) get extracting solution and add NaCl, under continuous stirring, saltout, placed 8-12 hour, filter and collect rock Rhizoma Coptidis alkaloid sulfate precipitation,
3) the alkaloid precipitation is dissolved in the ethanol, adds an amount of active carbon, the reflux decolouring is filtered, and the filtrate decompress(ion) concentrates and reclaims ethanol, and the concentrate drying product are rock Rhizoma Coptidis alkaloid.
The extracting method of 9 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 8 is characterized in that: it is an amount of 1) to get rock Rhizoma Coptidis plant herb, is crushed to coarse powder, adds 4~16 times of amount 0.1~1% aqueous sulfuric acids, and soak at room temperature extracted 24 hours, filter,
2) get extracting solution and add 10~20% NaCl, under continuous stirring, saltout, placed 8-12 hour, filter collection rock Rhizoma Coptidis alkaloid sulfate precipitation,
3) the alkaloid precipitation is dissolved in the ethanol of 20 times of weight, adds an amount of active carbon, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaims ethanol, and the concentrate drying product are rock Rhizoma Coptidis alkaloid.
1), get rock Rhizoma Coptidis plant herb the extracting method of 10 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 8 is characterized in that:, be crushed to coarse powder, add 10 times of amount 0.1~1% aqueous sulfuric acids, soak at room temperature extracted 24 hours, filter,
2), get extracting solution, under continuous stirring, add 1.5 times of weight NaCl, saltout, placed 10 hours, filter, collection obtains rock Rhizoma Coptidis alkaloid sulfate precipitation,
3), alkaloid precipitation is dissolved in 20 times of weight ethanol, add 1.25 times of weight active carbons, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrates and obtains rock Rhizoma Coptidis alkaloid dry product.
1), get rock Rhizoma Coptidis plant herb the extracting method of 11 salt Rhizoma Coptidis total alkaloids extracts as claimed in claim 8 is characterized in that:, be crushed to coarse powder, add 16 times of amount 0.1~1% aqueous sulfuric acids, soak at room temperature extracted 24 hours, filter,
2), get extracting solution, under continuous stirring, add 1.5 times of weight NaCl, saltout, placed 10 hours, filter, collection obtains rock Rhizoma Coptidis alkaloid sulfate precipitation,
3), alkaloid precipitation is dissolved in 20 times of weight ethanol, add 1.25 times of weight active carbons, reflux was decoloured in 30 minutes, filtered, and the filtrate decompress(ion) concentrates and reclaim ethanol, concentrates and obtains rock Rhizoma Coptidis alkaloid dry product.
12 1 kinds of compositionss comprise salt Rhizoma Coptidis total alkaloids extract and salt and pharmaceutically acceptable carrier among any one of the claim 1-7.
13 compositionss as claim 12 is characterized in that it being tablet, capsule, coated tablet, suspensoid, Emulsion, powder pin, transfusion, injection, powder, granule, drop pill, suppository, ointment, gel, membrane, liniment, aerosol, sustained-release preparation, transdermal absorption formulation, liposome.
14 1 kinds of compositionss comprise salt Rhizoma Coptidis total alkaloids extract and the salt thereof among any one of the claim 1-7 and medically treat hepatitis medicament arbitrarily.
15 compositionss as claim 14, wherein treat hepatitis medicament and be selected from the following material one or more: (a) suppress virus protein in conjunction with and/or the chemical compound of infection cell, comprise antibody and glucamine polysaccharide at virus itself; (b) suppress virus discharges and suppress viral function gene expression from virus coat chemical compound; (c) chemical compound of interfere with or compromise cellular replication; (d) chemical compound of change immunologic function; (e) play chemical compound and/or the plant extract that improves hepatitis symptom.
16 as claim 14 or 15 described compositionss, comprise salt Rhizoma Coptidis total alkaloids extract among any one of the claim 1-7 and salt thereof, medically treat hepatitis medicament and acceptable accessories arbitrarily.
17 1 kinds of test kits comprise salt Rhizoma Coptidis total alkaloids extract among any one of the claim 1-7 and salt thereof, medically treat hepatitis medicament arbitrarily and are loaded with the label of operation instructions.
18 as test kit as described in the claim 14, wherein treats hepatitis medicament and is selected from the following material one or more: (a) suppress virus protein in conjunction with and/or the chemical compound of infection cell, comprise antibody and glucamine polysaccharide at virus itself; (b) suppress virus discharges and suppress viral function gene expression from virus coat chemical compound; (c) chemical compound of interfere with or compromise cellular replication; (d) chemical compound of change immunologic function; (e) play chemical compound and/or the plant extract that improves hepatitis symptom.
The purposes of salt Rhizoma Coptidis total alkaloids extract product in preparation treatment hepatitis medicament that 19 claim 1-7,12-18 are any one.
20 purposes as claimed in claim 12, wherein hepatitis is viral hepatitis.
21 purposes as claimed in claim 13, wherein hepatitis is hepatitis B.
CNA2007100996879A 2007-05-29 2007-05-29 Corydalis saxicola total alkaloid, preparation method and uses thereof Pending CN101313939A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNA2007100996879A CN101313939A (en) 2007-05-29 2007-05-29 Corydalis saxicola total alkaloid, preparation method and uses thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNA2007100996879A CN101313939A (en) 2007-05-29 2007-05-29 Corydalis saxicola total alkaloid, preparation method and uses thereof

Publications (1)

Publication Number Publication Date
CN101313939A true CN101313939A (en) 2008-12-03

Family

ID=40105183

Family Applications (1)

Application Number Title Priority Date Filing Date
CNA2007100996879A Pending CN101313939A (en) 2007-05-29 2007-05-29 Corydalis saxicola total alkaloid, preparation method and uses thereof

Country Status (1)

Country Link
CN (1) CN101313939A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101874833A (en) * 2009-04-30 2010-11-03 成都中医药大学 Novel application of wine-roasted Chinese goldthread processed product
CN103548695A (en) * 2013-11-04 2014-02-05 广西壮族自治区药用植物园 Tissue culture and rapid propagation method for corydalis saxicola bunting
CN106290674A (en) * 2016-10-12 2017-01-04 广西河丰药业有限责任公司 The quality determining method of Corydalis saxicola Bunting injection
CN112656842A (en) * 2021-01-29 2021-04-16 广西河丰药业有限责任公司 Preparation method of corydalis saxicola bunting extract and corydalis saxicola bunting injection
CN114621362A (en) * 2021-12-06 2022-06-14 广西师范大学 Method for extracting high-purity polysaccharide from corydalis saxicola bunting
CN116813611A (en) * 2023-08-24 2023-09-29 云南省农业科学院生物技术与种质资源研究所 Preparation method and application of isoquinoline alkaloid

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101874833A (en) * 2009-04-30 2010-11-03 成都中医药大学 Novel application of wine-roasted Chinese goldthread processed product
CN103548695A (en) * 2013-11-04 2014-02-05 广西壮族自治区药用植物园 Tissue culture and rapid propagation method for corydalis saxicola bunting
CN103548695B (en) * 2013-11-04 2015-10-21 广西壮族自治区药用植物园 A kind of meadowrueleaf corydalis root quick breeding method for tissue culture
CN106290674A (en) * 2016-10-12 2017-01-04 广西河丰药业有限责任公司 The quality determining method of Corydalis saxicola Bunting injection
CN112656842A (en) * 2021-01-29 2021-04-16 广西河丰药业有限责任公司 Preparation method of corydalis saxicola bunting extract and corydalis saxicola bunting injection
CN114621362A (en) * 2021-12-06 2022-06-14 广西师范大学 Method for extracting high-purity polysaccharide from corydalis saxicola bunting
CN116813611A (en) * 2023-08-24 2023-09-29 云南省农业科学院生物技术与种质资源研究所 Preparation method and application of isoquinoline alkaloid
CN116813611B (en) * 2023-08-24 2023-12-01 云南省农业科学院生物技术与种质资源研究所 Preparation method and application of isoquinoline alkaloid

Similar Documents

Publication Publication Date Title
US20060233896A1 (en) Medicinal preparation containing phenylethanoid glycosides extracted from herbaceous plant, Cistanche tubulosa (Schenk.) Wight, process of making the same, and uses of the same
CN101313939A (en) Corydalis saxicola total alkaloid, preparation method and uses thereof
CN108530430B (en) Ester type catechin pyrrolidine alkaloid and preparation method and application thereof
CN101480422A (en) Tibetan oriental wormwood extract as well as preparation method and use thereof
CN102670631A (en) Olive total phenylethanoid glycoside composition and preparation and application thereof
CN101623469B (en) Detection method of Guwei collaterals-activating tincture
CN1989984B (en) Chuanxiong rhizome effective ingredient, preparing method, preparation and use thereof
CN101637550B (en) Chinese fanpalm seed polysaccharide extract and preparation method and purpose thereof
CN100444849C (en) New use of tribulus terrestris extraction
CN104224952A (en) Preparation method for total anthraquinones of rheum officinale with stable and uniform proportions of all components
CN103055191B (en) Preparation method and quality detection method of traditional Chinese medicine for treating hematuresis caused by nephritis
CN112791137B (en) Three shizandra berry extracts and preparation process and application thereof
CN108619374A (en) A kind of ginseng, fritillary bulb composition and its preparation method and application
CN105748652B (en) Serissa japonica capsule for treating gout and preparation method thereof
CN104398619A (en) Fevervine extract and applications thereof
CN103760271B (en) The detection method of brain heart clearing capsule
CN103877149A (en) Phospholipid complex containing dracocephalum moldavica total flavonoids, self-emulsifying agent prepared from same and preparation method of phospholipid complex containing dracocephalum moldavica total flavonoids
CN111329866A (en) Application of pentacyclic triterpenoid in preparation of anti-migraine medicine
CN104739923B (en) A kind of kidney tea total phenol and preparation method thereof for treating chronic nephritis
CN101249129B (en) Chinese medicine extract combination and medicine use thereof
CN100565202C (en) The detection method of medicine containing swertia psedochinensis and milk thistle silybum marianum
CN111568935B (en) Application of Siberian cocklebur fruit extract in preparation of antitumor drugs
CN1961895B (en) A novel anticancer pharmaceutical composition and preparation method thereof
CN108743654B (en) Traditional Chinese medicine composition for treating ischemic heart disease and preparation method and application thereof
EP1498131A1 (en) Medicinal preparation containing phenylethanoid glycosides extracted from Cistanche tubulosa

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Open date: 20081203