CN101849994B - Preparation method of macleaya cordata extracts - Google Patents
Preparation method of macleaya cordata extracts Download PDFInfo
- Publication number
- CN101849994B CN101849994B CN2009100430456A CN200910043045A CN101849994B CN 101849994 B CN101849994 B CN 101849994B CN 2009100430456 A CN2009100430456 A CN 2009100430456A CN 200910043045 A CN200910043045 A CN 200910043045A CN 101849994 B CN101849994 B CN 101849994B
- Authority
- CN
- China
- Prior art keywords
- herba macleayae
- macleayae cordatae
- extract
- sanguinarine
- alkali
- 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.)
- Active
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a preparation method of macleaya cordata extracts, which comprises the following steps: carrying out diacolation on macleaya cordata medical materials by an acid solution; adding alkali into diacolation liquid for regulating the solution to the alkaline solution for carrying out alkali deposition; dissolving precipitates by low-carbon alcohol; adding a proper amount of active carbon for back flowing extraction; adding acid for generating salt after the recovery of partial solvents from extraction liquid, and separating out orange crystalline precipitates; filtering the precipitates; using alcohol to wash remained acid; and obtaining the macleaya cordata extracts after drying. The extracts have the main ingredients of benzophen anthridine alkaloid salt with sanguinarine and chelerythrine as the representatives, and the total content is not lower than 60 percent through being metered by raw alkali, wherein the content of the sanguinarine is not lower than 40 percent, and the content of the chelerythrine is not lower than 18 percent. The preparation of the macleaya cordata extracts of the invention has the advantages of simple method and equipment, stable process, short production period and little environment pollution. The obtained extracts have high yield, low cost and stable product quality.
Description
Technical field
The present invention relates to a kind of method for preparing that is suitable for the Herba Macleayae Cordatae extract of suitability for industrialized production.
Technical background
Herba Macleayae Cordatae (Macleaya cordata (Willd) R.Br.) is a Papaveraceae Macleaya plant; Its main active is benzylisoquinoline class (benzylisoquinolines) alkaloid; Mainly contain benzo phenanthridines class (benzophenanthridines) alkaloid and protopines such as protopine, allocryptopine (protopines) alkaloids such as Sanguinarine, chelerythrine, 13-methyl-13,14-dihydro-[1,3, dihydrochelerythrine, wherein Sanguinarine and chelerythrine alkali content are higher.Traditional method is with the Herba Macleayae Cordatae all herbal medicine, but discovers, the content of benzo phenanthridine alkaloid is higher in the Herba Macleayae Cordatae fruit, can reach more than 1.5%.Report is arranged: in suitable collection period, the content of benzo phenanthridine alkaloid also can reach more than 1% in the leaf of Herba Macleayae Cordatae.
The documents and materials of relevant Herba Macleayae Cordatae extract technical study are a lot, relate to the following certain methods that mainly contains of total alkaloids extraction:
The hot lifting manipulation of sour water: like Hu Zhibi; Xu Yin etc. are in 1979 the 9th phases of Acta Pharmaceutica Sinica disclosed " research of effective ingredient in the Herba Macleayae Cordatae fruit ", and its technology is: dilute hydrochloric acid heat is carried, sour extract ammonia alkali deposited; Deposition soda acid repeated treatments, reuse silica gel separates with alumina column chromatography.This class methods hydrochloric acid and ammonia all are volatile substances, influence environmental protection; The soda acid repeated treatments, technology is loaded down with trivial details, and the cycle is long, and extraction ratio and yield are all lower; It is higher to carry out the separation of produced cost with silica gel and aluminium oxide, and treating capacity is less.The method that has the acid solution merceration to extract in addition, process cycle is long, extracts not exclusively.
Liquid-liquid extraction method: like the hair roc; Zhou Le etc. are agricultural 2004 the 2nd phases of journal disclosed " Macleaya cordata alkaloids extraction process preliminary study " in the northwest; It is solvent that its technology adopts chloroform, methanol and industrial alcohol respectively; Alkaloid in the Herba Macleayae Cordatae herb extracts, and gained extractum dissolving back adjust pH extracts respectively with chloroform.This type of procedure is complicated, operation is loaded down with trivial details, is not suitable for suitability for industrialized production; Total alkaloids constituents extraction ratio is low, solvent consumption is big, and production cost is high.
Macroporous resin partition method: like Li Jiancheng; He Lian; Liu Pingan is 2004 the 2nd phases of Journal of Traditional Chinese Medicine disclosed " enriching and purifying macroporous resin macleaya cordata total alkaloid technical study " in the Hunan; And for example strongly fragrantly build life, Yu Jianping is 2007 the 3rd phases of agricultural sciences disclosed " research of macroporous adsorbent resin separation and purification macleaya cordata total alkaloid " in Jiangsu.This class methods technology is more loaded down with trivial details, and solvent consumption is bigger, and product yield is not high, and production cost is higher.
Ultrasonic extraction: like Wang Xin, Zhou Le etc. are in northwest agricultural 2005 the 5th phases of journal disclosed " in the Herba Macleayae Cordatae alkaloidal supersound extraction with separate ", and these class methods are higher to equipment requirements, and industrially scalable production is still immature.
Liquid film separation and Extraction method: like Ma Ming; Liang Feng equals the disclosed patent of December in 2007 26 days " method of biosphere in the liquid film separation and Extraction Herba Macleayae Cordatae ", and (application number is 200710035400.6; Publication number is CN101091748A), its technology is made surfactant for to make membrane solvent with edible oil with Span80; Phosphoric acid fat is made carrier; Extracting solution and the emulsion of Herba Macleayae Cordatae sour water supersound extraction gained pH=4 are pressed the whey volume ratio for stirring extraction in (50: 5～50: 20) adding extractor, and the heating in water bath breakdown of emulsion divides oil-yielding stratum, and water is the solution of total alkaloids in the Herba Macleayae Cordatae.The reagent that these class methods need be used is various, consumes bigger; Technology relates to supersound extraction, water-bath, and emulsifying when extracting the emulsion proportion very big, so disposal ability is limited, is difficult for realizing industrially scalable production.
The acidic ethanol extraction method: like Li Hui, Xiao Shangjia is 2008 the 19th phases disclosed " Study on extraction of Herba Macleayae Cordatae medical material " in the Chinese Medicine Leader, and its technology is that the Herba Macleayae Cordatae medical material extracts with 80% ethanol, adjusting pH=5.0,60 ℃ of warm macerating.This class methods ethanol consumption is big, cost is high, and extract obtained content is lower.
Summary of the invention:
The object of the present invention is to provide and a kind ofly use that equipment is simple, process stabilizing, with short production cycle, environmental pollution is little, be suitable for the method for preparing of the Herba Macleayae Cordatae extract of industrialized great production; This method prepares gained Herba Macleayae Cordatae extract yield height, low, the constant product quality of cost simultaneously.
The Herba Macleayae Cordatae medical material is carried out hot percolation with acid solution; Percolate adds adjusting PH with base value to 9～10 and carries out alkali deposited; Deposition is carried out reflux, extract, with low-carbon alcohols dissolving and adding active carbon; Add acid behind the extracting solution recovery section solvent and become to salt out crystalline precipitate, deposition is with promptly getting Herba Macleayae Cordatae extract after the residual sour drying of pure flush away.
Described Herba Macleayae Cordatae medical material is the dry mature fruit of Papaveraceae Macleaya plant Herba Macleayae Cordatae or the leaf of Herba Macleayae Cordatae of the suitable state of gathering, or both mixture.
The Herba Macleayae Cordatae medical material that described Herba Macleayae Cordatae medical material also can be selected the different places of production for use adopts the assorted mode that feeds intake behind the content that detects Sanguinarine and chelerythrine, make in the raw material ratio of Sanguinarine and chelerythrine be 2～2.5 (guaranteeing as far as possible that also Sanguinarine and the two ratio of chelerythrine were near 2: 1 in the extract).
Described acid solution is dilute sulfuric acid, hydrochloric acid or the phosphoric acid of concentration 0.4～1%; But be preferably 0.4～1% dilution heat of sulfuric acid, its hot percolation temperature preferably is not less than 45 ℃, is not higher than 100 ℃.
Described percolate adds alkali and transfers to meta-alkalescence and carry out alkali deposited, and its alkali is meant NaOH, KOH, Ca (OH)
2But be that calcium hydroxide transfers to meta-alkalescence especially with the lime cream of washing by quicklime.
Described low-carbon alcohols is meant ethanol or methanol.
Describedly add acid and carry out salify, its acid is meant concentrated sulphuric acid or concentrated hydrochloric acid or SPA, and adjust pH is 1～3.
The content of total alkali or salt is in Sanguinarine or salt and chelerythrine or salt, the benzo phenanthridines class total alkaloids or the mass percent of salt in extract that adopt the HPLC method to measure.It is said if what use that the concentrated sulphuric acid salify obtains is that the disulfate of Sanguinarine and chelerythrine is the benzo phenanthridines class total alkaloids disulfate of leading.Benzo phenanthridines class total alkaloid content is not less than 60% in former alkali, and wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%; Benzo phenanthridines class total alkaloids salt content is not less than 77%.Saidly be not less than 60% if what use that the concentrated hydrochloric acid salify obtains is to be master's benzo coffee pyridine class total alkaloids hydrochlorate with Sanguinarine chloride and chlorination chelerythrine in former alkali total content, wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%; Benzo phenanthridines class total alkaloids salt content is not less than 66%; It is said if what use that the SPA salify obtains is to be master's benzo phenanthridines class total alkaloids dihydric phosphate with Sanguinarine dihydric phosphate and chelerythrine dihydric phosphate; Wherein Sanguinarine is not less than 40%; Chelerythrine is not less than 18%, and benzo phenanthridines class total alkaloids dihydric phosphate is not less than 77%.
The inventor proves also that through experiment there is less stable in the benzo phenanthridine alkaloid with former alkali form; Therefore; In fact this extract manufactures the Herba Macleayae Cordatae extract that exists with benzo phenanthridine alkaloid salt form; Mainly as medical product, the raw material of veterinary drug medicated feed additive or veterinary drug injection and botanical pesticide.
Problem such as the invention solves suitability for industrialized production Herba Macleayae Cordatae extract complex process, solvent consumption is big, cost is high, yield is low, the present invention has guaranteed the product quality of Herba Macleayae Cordatae extract.
The present invention has adopted the form of hot percolation, and the method that adopts hot percolation to extract to the Herba Macleayae Cordatae medical material does not have reported in literature so far as yet.The present invention make that whole technology is simple and direct, and equipment is simple through adopting the mode of hot percolation, and extraction ratio is high, and improve the yield of Herba Macleayae Cordatae extract product greatly, thereby reduced production cost, and suitable suitability for industrialized production.The Herba Macleayae Cordatae extraction process of existing bibliographical information, total alkali (in 60%) yield is general 0.5～1%, and through process recovery ratio of the present invention generally more than 1% even be higher than 1.5%.The utilization rate of resource is improved more than 50%, very meaningful to economizing on resources.In addition; What adopt in the technology of the present invention is activated carbon adsorption; Regular meeting brings some exogenous noxious substances into because of raw material in the extract; Like benzopyrene, dioxin etc., this is because plant affected by environment or influence of supplementary material and packaging material etc. in growth course all possibly cause can introducing these noxious substances in the extract.The inventor finds that through a large amount of experimentation active carbon has removal effect preferably to these noxious substances, thus the present invention to add in the alcohol extraction process that active carbon removes be necessary.The inventor is through comparing experiment, the result show: Yi the bioxin be the toxic equivalent of example Qi bioxin of extract of not adding the activated carbon gained sometimes greater than 200ppt, and add activated carbon extract obtained two dislike because of toxic equivalent often less than 1ppt.
In addition; Also preferred employing of inventor selects for use dilute sulfuric acid " percolation " as optimized mode; Because hydrochloric acid has volatility, the possibility contaminated air also possibly cause corrosion to equipment during percolation; Sulphuric acid is easy to get than phosphoric acid is more convenient, so the hot dilute sulfuric acid solution of process using of the present invention carries out the percolation extraction as optimal condition.Calcium hydroxide alkali deposited: because when using dilute sulfuric acid or phosphoric acid percolation; If use sodium hydroxide or potassium hydroxide alkali deposited; Sulfate radical or phosphate anion bring very burden with a large amount of being discharged in the environment of the form of water solublity sodium salt or potassium salt to next step environmental protection treatment.Therefore the inventor selects for use calcium hydroxide to carry out alkali deposited, has also precipitated most sulfate radicals and phosphate anion in the assurance abundant sedimentary while of alkaloid like this, helps environmental protection treatment.
In order further to make constant product quality of the present invention; The inventor preferably adopted the assorted mode that feeds intake scientific and reasonable utilize herb resource; And through having determined Sanguinarine and chelerythrine ratio are 1.8～2.5: 1 (and as far as possible near 2: 1) in the raw material; Can be so that total alkaloid contents be not less than 60% in former alkali in the extract, wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%.Raw material and extract detect its total alkaloid contents as marker ingredients with HPLC with Sanguinarine and chelerythrine.
The inventor has also worked out the content HPLC detection method in the benzo phenanthridines class total alkaloids or the salt of Sanguinarine or salt and chelerythrine or salt.Basic skills is following: it is an amount of that precision takes by weighing the test sample powder, place in the 50ml volumetric flask, and with methanol-1% phosphoric acid water (50: 50) dissolving, ultrasonic 45min, cooling standardize solution.Filtering with microporous membrane with 0.45 μ m is subsequent use.Mobile phase: acetonitrile+0.1% phosphoric acid water=30+70 (V/V) (adding 0.1ml phosphoric acid in every 100ml water); Flow velocity: 1.0ml/min; Column temperature: 35 ℃; Detect wavelength: 270nm; Sampling volume: 5 μ l, detect under this condition.With Sanguinarine chloride, chlorination chelerythrine do standard reference material calculate Sanguinarine and the total former alkali of chelerythrine with and hydrochlorate or disulfate or the mass percent of dihydric phosphate in extract.
The mass percent of total alkaloids is not less than 60% in former alkali in the extract, and wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%; According to the molecular weight mass percent of its salt in extract that can convert: with the hydrochlorate timing; The content of Sanguinarine hydrochloride is not less than 44.27%; The content of chelerythrine hydrochlorate is not less than 19.84%; The content of total alkaloids hydrochlorate is not less than 66% (be not less than 60% by total alkali and convert, the result rounds up and promptly gets 66%); With the disulfate timing; The content of Sanguinarine disulfate is not less than 51.67%; The content of chelerythrine disulfate is not less than 23.01%, and the content of total alkaloids disulfate is not less than 77% (be not less than 60% by total alkali and convert, the result rounds up and promptly gets 77%); With the dihydric phosphate timing; The content of Sanguinarine dihydric phosphate is not less than 51.67%; The chelerythrine dihydric phosphate is not less than 23.01%, and the total alkaloids dihydric phosphate is not less than 77% (be not less than 60% by total alkali and convert, the result rounds up and promptly gets 77%).The Herba Macleayae Cordatae extract of existing bibliographical information is not generally set the index that total alkaloid content is not less than 60% (comprise that Sanguinarine is not less than 40%, chelerythrine is not less than 18%).Inventor's purport is through this patent of invention, and the product that industrial-scale production is obtained is metastable, thereby has formulated this indication range.
The present invention includes following implementation step:
(1) hot percolation: with the Herba Macleayae Cordatae medical material with 10 times～30 times amounts, 45～100 ℃ 0.4～1% dilution heat of sulfuric acid percolation;
(2) alkali deposited: in the lime cream of washing with quicklime with percolate and transfer to pH=9～10;
(3) deposition alcohol extraction: deposition is with alcohol reflux 2 times, and quantity of solvent is 8～10 times of amounts of precipitation capacity, and the adding active carbon, extracts 1～2 hour at every turn;
(4) salify: add concentrated sulphuric acid behind the ethanol extract recovery section etoh solvent and transfer pH=1～3 to carry out salify, gained salmon pink deposition promptly gets benzo phenanthridines total alkali disulfate with the residual sour after drying of pure flush away and is not less than 77% Herba Macleayae Cordatae extract.
Select for use the hydrochloric acid salify to obtain the extract of chlorination Herba Macleayae Cordatae benzo phenanthridines total alkali salt; Select for use the sulphuric acid salify to obtain the extract of Herba Macleayae Cordatae benzo phenanthridines class total alkaloids disulfate; Select for use the phosphoric acid salify to obtain the extract of Herba Macleayae Cordatae benzo phenanthridines class total alkaloids dihydric phosphate.But no matter be with which kind of salify mode; It is that the benzo phenanthridines class total alkaloids of representative is with former alkali mass percent >=60% in Sanguinarine and chelerythrine; Sanguinarine >=40% wherein; Chelerythrine >=18%, prescription are consistent, but the mass percent of different salt in extract differs bigger.Therefore, when working out the Herba Macleayae Cordatae extract quality standard and measuring its content, be the best with former alkali representative products quality in principle.
The conclusive evidence of benzo phenanthridine alkaloid and sulphuric acid and phosphoric acid salify product: benzo phenanthridine alkaloid composition main in the Herba Macleayae Cordatae is mainly Sanguinarine and chelerythrine.Obtain Sanguinarine chloride and chlorination chelerythrine with the hydrochloric acid salify, this is clear and definite; What obtain with the sulphuric acid salify is Sanguinarine disulfate and chelerythrine disulfate, and this point inventor studies conclusive evidence through following experiment:
Get high-purity Sanguinarine (98%), the alcohol reflux dissolving with 95% is divided into 2 parts, and portion adds the concentrated sulphuric acid salify and must precipitate, and deposition gets A 2 times with 95% ethyl alcohol recrystallization
1, precision takes by weighing A
1Be dissolved in the distilled water, add and analyze about pure cerium hydroxide sodium accent pH=9, leave standstill, sucking filtration must precipitate, and deposition gets A with an amount of distilled water wash after drying to constant weight
2, precision is weighed; Portion adds the concentrated hydrochloric acid salify and must precipitate, and deposition gets B 2 times with 95% ethyl alcohol recrystallization
1Precision takes by weighing B
1Be dissolved in the distilled water, add and analyze about pure cerium hydroxide sodium accent pH=9, leave standstill, sucking filtration must precipitate, and deposition gets B with an amount of distilled water wash after drying to constant weight
2, precision is weighed.
Known:
Sanguinarine molecular weight M [C
20H
14NO
4] be: 332.33
Sanguinarine hydrochloride molecular weight M [C
20H
14NO
4Cl] be: 367.83
If its molecular weight of sanguinarine sulfate M is [C
20H
14NO
4 +1/2 (SO
4 2-)] be: 380.33
If its molecular weight of Sanguinarine disulfate M is [C
20H
14NO
4HSO
4] be: 429.33
M[C
20H
14NO
4·Cl]/M[C
20H
14NO
4]＝1.1068
M[C
20H
14NO
4 +·1/2(SO
4 2-)]/M[C
20H
14NO
4]＝1.1444
M[C
20H
14NO
4·HSO
4]/M[C
20H
14NO
4]＝1.2919
Through repeated experiments repeatedly, gained B
1/ B
2Value and 1.1068 coincide gained A
1/ A
2Value and 1.2919 coincide and with 1.1444 misfit, so Sanguinarine and the salifiable product of sulphuric acid are [C
20H
14NO
4HSO
4].Same method confirms to such an extent that chelerythrine and the salifiable product of sulphuric acid are [C
21H
18NO
4HSO
4].Being standard substance with the chloride through HPLC in addition carries out analytical test and converts that also should to demonstrate,prove the salifiable product of benzo phenanthridine alkaloid and sulphuric acid be disulfate sample size.Same method conclusive evidence benzo phenanthridine alkaloid and the salifiable product of phosphoric acid are dihydric phosphates.
The specific embodiment:
Following examples are intended to explain the present invention rather than to further qualification of the present invention.
Embodiment 1:
Get Anhui and produce Herba Macleayae Cordatae fruit 1000g, 0.5% sulfuric acid solution that is not less than 80 ℃ with 10L carries out percolation, and percolate adds sodium hydroxide and transfers the pH=10 alkali deposited; Gained deposition is with 95% alcohol reflux 2 times; Add ethanol 1L the 1st time, add the proper amount of active carbon powder, refluxed 2 hours; Add ethanol 0.8L the 2nd time, add active carbon powder, refluxed 1 hour; Merge ethanol extract twice, in concentrated solution, add concentrated sulphuric acid while stirring when concentrate reclaiming ethanol and transfer pH=3, cross and filter salmon pink and precipitate to about 0.8L; Deposition is clean with pickling with ethanol; Be drying to obtain Herba Macleayae Cordatae extract 11.8g, total alkaloid content is 69.56% (Sanguinarine content is 46.54%, and the chelerythrine alkali content is 23.02%).
Embodiment 2:
Get Anhui and produce Herba Macleayae Cordatae fruit 600g, total alkaloid content is 1.68% (Sanguinarine content is 1.13%, and the chelerythrine alkali content is 0.55%); Other gets Guangxi and produces Herba Macleayae Cordatae fruit 400g, and total alkaloid content is 1.14% (Sanguinarine content is 0.73%, and the chelerythrine alkali content is 0.41%); Two parts of raw materials are fully mixed, be not less than 50 ℃ 0.5% hydrochloric acid solution percolation with 20L, percolate adds potassium hydroxide and transfers the pH=9 alkali deposited; Gained deposition is with alcohol reflux 2 times; Add 90% ethanol 1L the 1st time, add active carbon powder, refluxed 2 hours; Add 90% ethanol 0.8L the 2nd time, add active carbon powder, refluxed 2 hours; Merge alcohol extract twice, concentrate recovery ethanol to concentrated solution volume and be about 0.8L, in concentrated solution, add concentrated hydrochloric acid while stirring and transfer pH=2; Cross and filter salmon pink deposition, precipitate pickling is only, be drying to obtain Herba Macleayae Cordatae extract 12.5g with ethanol; Total alkaloid content is 63.35% (Sanguinarine content is 42.14%, and the chelerythrine alkali content is 21.21%).
Embodiment 3:
Get Guangxi and produce Herba Macleayae Cordatae fruit 1000g, with the phosphoric acid solution percolation of 60 ℃ 0.8% of 20L, percolate adds calcium hydroxide and transfers the pH=10 alkali deposited, and gained precipitates reflux, extract, 2 times, adds methanol 1.5L the 1st time, adds active carbon powder, refluxes 2 hours; Add methanol 1.2L the 2nd time, add active carbon powder, refluxed 1 hour; Merge alcohol extract twice, concentrate recovery methanol to concentrated solution volume and be about 1L, in concentrated solution, add SPA while stirring and transfer pH=1; Cross and filter salmon pink deposition, precipitate pickling is only, be drying to obtain Herba Macleayae Cordatae extract 10.5g with methanol; Total alkaloid content is 64.91% (Sanguinarine content is 44.77%, and the chelerythrine alkali content is 20.14%).
Embodiment 4:
Get the Hunan and produce Herba Macleayae Cordatae fruit 1000g, be not less than 80 ℃ 0.5% sulfuric acid solution percolation with 20L, percolate adds calcium hydroxide and transfers the pH=9 alkali deposited, and gained deposition reflux, extract, 2 times adds 90% ethanol 1.6L the 1st time, adds the proper amount of active carbon powder, refluxes 2 hours; Add 90% ethanol 1.3L the 2nd time, add active carbon powder, refluxed 2 hours; Merge alcohol extract twice, concentrate recovery ethanol to concentrated solution volume and be about 1L, in concentrated solution, add concentrated sulphuric acid while stirring and transfer pH=2; Cross and filter the salmon pink deposition, deposition gets Herba Macleayae Cordatae extract 15.6g with ethanol with sour cleaning, drying; Total alkaloid content is 66.53% (Sanguinarine content is 45.51%, and the chelerythrine alkali content is 21.02%).
Claims (11)
1. the method for preparing of a Herba Macleayae Cordatae extract; It is characterized in that: the Herba Macleayae Cordatae medical material is carried out hot percolation with acid solution; Percolate adds adjusting PH with base value to 9～10 and carries out alkali deposited; Deposition is carried out reflux, extract, with low-carbon alcohols dissolving and adding active carbon, adds acid behind the extracting solution recovery section solvent and becomes to salt out crystalline precipitate, and deposition is with promptly getting Herba Macleayae Cordatae extract after the residual sour drying of pure flush away; 45 ℃≤hot percolation temperature≤100 ℃; Described acid solution is 0.4～1% dilute sulfuric acid, hydrochloric acid or phosphoric acid; Alkali in the said alkali deposited is meant NaOH, KOH or Ca (OH)
2.。
2. the method for preparing of a kind of Herba Macleayae Cordatae extract according to claim 1, it is characterized in that: described acid solution is a dilute sulfuric acid.
3. according to the method for preparing of claims 1 or 2 described a kind of Herba Macleayae Cordatae extract, it is characterized in that: what the alkali in the said alkali deposited was used is the lime cream that quicklime is washed.
4. according to the method for preparing of claims 1 described a kind of Herba Macleayae Cordatae extract, it is characterized in that: describedly add acid and carry out that employed acid is meant concentrated sulphuric acid or concentrated hydrochloric acid or SPA in the salification process, and adjust pH is 1～3.
5. according to the method for preparing of claims 1 described a kind of Herba Macleayae Cordatae extract; It is characterized in that: the Herba Macleayae Cordatae medicinal raw material that described Herba Macleayae Cordatae can be selected the different places of production for use is the assorted mode that feeds intake of employing behind the content that detects Sanguinarine and chelerythrine, makes that Sanguinarine and the two ratio of chelerythrine are 1.8～2.5: 1 in the raw material.
6. according to the method for preparing of claims 4 or 5 described a kind of Herba Macleayae Cordatae extract, it is characterized in that: what adopt that the concentrated sulphuric acid salify obtains is that disulfate with Sanguinarine and chelerythrine is master's a benzo phenanthridines class total alkaloids disulfate; Benzo phenanthridines class total alkaloid content is not less than 60% in former alkali, and Sanguinarine is not less than 40%, and chelerythrine is not less than 18%.
7. according to the method for preparing of claims 4 or 5 described a kind of Herba Macleayae Cordatae extract; It is characterized in that: described benzo phenanthridines total alkaloid salt is characterized in that: what employing concentrated hydrochloric acid salify obtained is to be master's benzo coffee pyridine class total alkaloids hydrochlorate with Sanguinarine chloride and chlorination chelerythrine; Benzo coffee pyridine class total alkaloid content is not less than 60% in former alkali, and wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%.
8. according to the method for preparing of claims 4 or 5 described a kind of Herba Macleayae Cordatae extract, it is characterized in that:, what the employing SPA obtained is to be master's benzo phenanthridine alkaloid hydrochloric acid dihydric salt with Sanguinarine dihydric phosphate and chelerythrine dihydric phosphate; Benzo coffee pyridine class total alkaloid content is not less than 60% in former alkali, and wherein Sanguinarine is not less than 40%, and chelerythrine is not less than 18%.
9. according to the method for preparing of claims 1 described a kind of Herba Macleayae Cordatae extract, it is characterized in that: described low-carbon alcohols is meant ethanol or methanol.
10. according to the method for preparing of claims 1 described a kind of Herba Macleayae Cordatae extract, it is characterized in that: described Herba Macleayae Cordatae medical material is the dry mature fruit of Papaveraceae Macleaya plant Herba Macleayae Cordatae, or leaf of Herba Macleayae Cordatae or both mixture.
11. the method for preparing according to claims 1 described a kind of Herba Macleayae Cordatae extract is characterized in that: (1) hot percolation: with the Herba Macleayae Cordatae medical material with 10 times～30 times amounts, 45～100 ℃ 0.4～1% dilution heat of sulfuric acid percolation;
(2) alkali deposited: in the lime cream of washing with quicklime with percolate and transfer to pH=9～10;
(3) deposition alcohol extraction: deposition is with alcohol reflux 2 times, and quantity of solvent is 8～10 times of amounts of precipitation capacity, and the adding active carbon, extracts 1～2 hour at every turn;
(4) salify: add concentrated sulphuric acid behind the ethanol extract recovery section etoh solvent and transfer pH=1～3 to carry out salify, gained salmon pink deposition promptly gets benzo phenanthridines total alkali disulfate with the residual sour after drying of pure flush away.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100430456A CN101849994B (en) | 2009-04-03 | 2009-04-03 | Preparation method of macleaya cordata extracts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100430456A CN101849994B (en) | 2009-04-03 | 2009-04-03 | Preparation method of macleaya cordata extracts |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101849994A CN101849994A (en) | 2010-10-06 |
| CN101849994B true CN101849994B (en) | 2012-07-04 |
Family
ID=42801783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100430456A Active CN101849994B (en) | 2009-04-03 | 2009-04-03 | Preparation method of macleaya cordata extracts |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101849994B (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617583B (en) * | 2012-03-08 | 2013-12-25 | 西北农林科技大学 | Method for quickly extracting and separating five types of alkaloids from macleaya cordata |
| CN104547050A (en) * | 2014-12-26 | 2015-04-29 | 湖南理工学院 | Application of macleaya cordata total alkaloids as external spermicide |
| CN108635422B (en) * | 2018-07-24 | 2021-02-09 | 湖南美可达生物资源股份有限公司 | Composition for preventing and treating respiratory diseases of livestock and poultry and preparation method thereof |
| CN108837006B (en) * | 2018-07-24 | 2021-04-06 | 湖南美可达生物资源股份有限公司 | Macleaya cordata leaf extract and preparation method and product thereof |
| CN108840874A (en) * | 2018-09-18 | 2018-11-20 | 湖北博瑞生物科技股份有限公司 | A kind of extracting method of sanguinarine |
| CN109526738B (en) * | 2018-12-13 | 2021-10-01 | 湖南美可达生物资源股份有限公司 | Method for inducing and promoting expression of macleaya cordata P6H gene and DBOX gene by combination of elicitor and mechanical injury |
| CN109496865B (en) * | 2018-12-13 | 2020-12-15 | 湖南美可达生物资源股份有限公司 | Induction medium and method for improving content of macleaya cordata sanguinarine and chelerythrine |
| CN110590463B (en) * | 2019-10-25 | 2021-10-15 | 湖北大学 | Fertilizer and molluscicide double-effect organic fertilizer molluscicide, preparation method and application thereof |
| CN112022964A (en) * | 2020-10-09 | 2020-12-04 | 杨大华 | Traditional Chinese medicine composition for preventing and treating cervical cancer and preparation method thereof |
| CN113519561B (en) * | 2021-06-10 | 2022-05-06 | 广州普邦园林股份有限公司 | Deinsectization egg composition for soil improvement and application thereof |
| CN117958282B (en) * | 2024-02-01 | 2024-06-25 | 安徽中医药大学 | Macleaya cordata extract and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740175A (en) * | 2005-08-29 | 2006-03-01 | 长沙世唯科技有限公司 | Plumepoppy total alkaloid salt and its prepn and application |
-
2009
- 2009-04-03 CN CN2009100430456A patent/CN101849994B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740175A (en) * | 2005-08-29 | 2006-03-01 | 长沙世唯科技有限公司 | Plumepoppy total alkaloid salt and its prepn and application |
Non-Patent Citations (2)
| Title |
|---|
| 李慧，肖佳尚.博落回药材的提取工艺研究.《中国医药导报》.2008,第5卷(第19期),11－13. * |
| 杨军衡,毛小环,陈爱军.中药博落回生物碱提取新工艺研究.《湖南环境生物职业技术学院学报》.2006,第12卷(第三期),274-277. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101849994A (en) | 2010-10-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101849994B (en) | Preparation method of macleaya cordata extracts | |
| CN101433565A (en) | Total alkaloid extract of seeds of harmel genus and effective monomer component thereof, and preparation and use thereof | |
| CN102285982B (en) | Method for separating and purifying monomer compounds from Chinese medicinal herb rhizoma coptidis | |
| CN101829201B (en) | Method for extracting alkaloid from monkshood medicinal material | |
| CN102001947A (en) | Method for preparing honeysuckle chlorogenic acid | |
| CN102285994B (en) | Method for separating and purifying fangchinoline and tetrandrine from stephania tetrandra | |
| CN101928285A (en) | Method for extracting major alkaloids from rhizoma coptidis | |
| CN105254500A (en) | Method for preparing high-purity chlorogenic acid from eucommia ulmoides leaf crude extract | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN101108871A (en) | Technique for extracting cycli phosphate adenosine from chinese date | |
| CN105753917A (en) | Separating purifying method of liquiritin | |
| CN104418743A (en) | Method for refining chlorogenic acid from honeysuckle crude extract | |
| CN102617583B (en) | Method for quickly extracting and separating five types of alkaloids from macleaya cordata | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN101851221B (en) | Method for preparing dihydroquercetin from larches | |
| CN104311616A (en) | Method for extracting high-purity esculine and fraxin from Cortex Fraxini | |
| CN101278989B (en) | Method for extracting Thalictrum aquilegifolium total alkaloids and total saponins from Thalictrum aquilegifolium | |
| CN101412724B (en) | Method for extracting bilobalide compound from ginkgo leaf | |
| CN105131005A (en) | Preparation method for high content macleaya cordata alkaloid | |
| CN102552122B (en) | Method for preparing sinomenine hydrochloride injection | |
| CN104370814B (en) | A kind of method extracting glaucine from the celestial rope of bundle | |
| CN102824473A (en) | Lycium ruthenicum murr total flavonoid extract and preparation method thereof | |
| CN102836280A (en) | Folium Lycii total flavone extract and preparation method thereof | |
| CN104072504A (en) | Method for extracting and purifying hernandia nymphaeifolia alkali from hernandia nymphaeifolia | |
| CN105348338A (en) | Method for extracting and separating paederosidic acid from Saprosma merrillii Lo |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: CENG JIANGUO Free format text: FORMER OWNER: HUNAN CHINESE MEDICINE EXTRACTION ENGINEERING RESEARCH CENTER, LTD. Effective date: 20150825 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20150825 Address after: 1, 2901, Hua Ya garden, Merrill Lynch street, Yuhua District, Hunan, Changsha 410000, China Patentee after: Zeng Jianguo Address before: 410331 Liuyang City, Hunan province Liuyang biomedical park Zhiyuan Road No. 27 Patentee before: Hunan Chinese Medicine Extraction Engineering Research Center, Ltd. |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160201 Address after: 410000 room 1, building 2901, Hua Ya garden, Merrill Lynch street, Yuhua District, Hunan, Changsha Patentee after: Shiwei Science and Technology Co., Ltd., Changsha Address before: 1, 2901, Hua Ya garden, Merrill Lynch street, Yuhua District, Hunan, Changsha 410000, China Patentee before: Zeng Jianguo |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160415 Address after: Kang Road, 410331 Hunan Province, Liuyang economic and Technological Development Zone No. 190 Patentee after: Hunan Micolta Bioresource Inc. Address before: 410000 room 1, building 2901, Hua Ya garden, Merrill Lynch street, Yuhua District, Hunan, Changsha Patentee before: Shiwei Science and Technology Co., Ltd., Changsha |
|
| C56 | Change in the name or address of the patentee | ||
| CP03 | Change of name, title or address |
Address after: Kang Road, 410311 Hunan Province, Liuyang economic and Technological Development Zone No. 190 Patentee after: Hunan meikeda biological Tiomin Resources Inc Address before: Kang Road, 410331 Hunan Province, Liuyang economic and Technological Development Zone No. 190 Patentee before: Hunan Micolta Bioresource Inc. |