CN109485652A - The Extraction and enrichment technique and its application of radix dactylicapni Protopine Protopine monomer - Google Patents
The Extraction and enrichment technique and its application of radix dactylicapni Protopine Protopine monomer Download PDFInfo
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Abstract
The invention discloses a kind of Extraction and enrichment techniques of radix dactylicapni Protopine Protopine monomer, include the following steps: to take appropriate radix dactylicapni medicinal material dry product, it crushes, it is put in extractor, addition is equivalent to the aqueous solution of 10 ~ 20 times of weight of radix dactylicapni medicinal material dry product amounts, stirs and steeped overnight, next day discard maceration extract, it is added in the dregs of a decoction and is equivalent to 8 ~ 13 times of weight of radix dactylicapni medicinal material dry product 9 ~ 10% aqueous acids measured, circumfluence distillation 2 ~ 5 times.The invention also discloses application of the radix dactylicapni Protopine Protopine monomer in relieving cough and asthma preparation, analgesia preparation, anti-arrhythmia preparation or anti-tumor agent.Technique of the invention is suitble to the Extraction and enrichment purifying of radix dactylicapni Protopine, and Biflorine purity is up to 80% or more, and further up to 95% or more after purification, the operating procedure of entire technique is simple and easy, and high income is at low cost.
Description
Technical field
The present invention relates to the Extraction and enrichment techniques and its application of a kind of radix dactylicapni Protopine Protopine monomer, belong to
In technical field of traditional Chinese medicines.
Background technique
Radix dactylicapni, Dactylicapnos scandens (D. Don) Hutch. are Dactylicapnos plant radix dactylicapni
Dry root.Autumn harvesting.Slice dries.It is radix dactylicapni bitter, cool in nature, have the effect of analgesia, hemostasis, anti-inflammatory, decompression, once by " in
State's pharmacopeia " version was recorded 1977 years.Pharmacological experiment confirms that alkaloid is that it has the main active of the pharmacological actions such as analgesia,
Wherein the isoquinoline alkaloids such as capaurine, isocorydine, Biflorine and cucoline are main components therein.
Capaurine, the content of isocorydine are higher in radix dactylicapni, are all larger than 1%, and the content of radix dactylicapni Protopine is about
0.1% is accounted for, Biflorine, Protopine is a kind of chemical substance, molecular formula C20H19O5N, molecular weight 353.37.Former Ah
Piece alkali has the effects that analgesia, inhibits platelet aggregation, loose smooth muscle, anti-arrhythmia, antitumor, anti-liver injury, simultaneously
There are also stronger anticholinesterase (anti-ACHE) activity and to cardiovascular remarkable effect.
It is found through clinical research, the main effective active composition of radix dactylicapni is Biflorine, from current document report it is found that existing
There is the synthetic method yield of Biflorine lower, some synthetic route higher costs are unsuitable for the acquisition of a large amount of Biflorines, because
This, to Biflorine extract process of enriching research be it is necessary to and also it is very important.
The Extraction and enrichment method of Biflorine is generally obtained by taking alcohol extracting to corydalis tuber medicinal material at present, and research is found
The optimised process that total corydaline extracts are as follows: concentration of alcohol 50%, 7 times of ethanol consumption, ultrasonic extraction 45min.Extraction process behaviour
Make simply, it is reproducible.And contain tetrahydropalmatine and Biflorine in rhizoma corydalis, the content of tetrahydropalmatine is about 0.06%,
Biflorine content is about 0.03%, and the polarity of tetrahydropalmatine is slightly larger than Biflorine, and it is difficult to there is separation therebetween
The problem of.In addition, since solution that alcohol extract condenses in concentration process is not the alcoholic solution of corresponding proportion, therefore alcohol recycles
Liquid is every time using adjusting determining alcohol is both needed to, and there are troublesome in poeration, at high cost, the big problems of solvent consumption.In conclusion at present
Preparation process flow of the Biflorine without specification, the production cycle is long, and reagent waste is serious and is difficult to ensure the yield of Biflorine
And purity, to significantly limit application of the Biflorine in terms of medicine.Through literature survey there is not yet from radix dactylicapni
Extract the report of separating high-purity Biflorine.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of mentioning for radix dactylicapni Protopine Protopine monomer
Process of enriching is taken, the stable technical process, environmental-friendly, simple and easy to do, the Biflorine of purity >=80%, pole has been made in separation
The medicinal utility value of radix dactylicapni is improved greatly；Further, the present invention provides a kind of radix dactylicapni Protopine Protopine
The Extraction and enrichment technique of monomer, the method can effectively separate capaurine, isocorydine with Biflorine, and purity >=95% is made
Biflorine, Biflorine purity is high, yield > 55%.The present invention also provides a kind of radix dactylicapni Protopine Protopine
Application of the monomer in relieving cough and asthma preparation, analgesia preparation, anti-arrhythmia preparation or anti-tumor agent, is greatly enriched original
Application of the opium alkali in terms of medicine.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows:
The Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer includes the following steps: to take appropriate radix dactylicapni medicinal material
Dry product is crushed, is put in extractor, and the aqueous solution for being equivalent to 10 ~ 20 times of weight of radix dactylicapni medicinal material dry product amounts is added, stirs and soaks
Stain is stayed overnight, and next day discards maceration extract, and 9 ~ 10% acid for being equivalent to 8 ~ 13 times of weight of radix dactylicapni medicinal material dry product amounts is added in the dregs of a decoction
Aqueous solution, circumfluence distillation 2 ~ 5 times, each extraction time is 1 ~ 3h, and Extracting temperature is 70 ~ 80 DEG C, merges acid water extracting liquid, dense
When the density for being reduced to extraction concentrate is 1.08 ~ 1.15, stop concentration, filter, cationic exchange resin adsorption is added in filtrate
Total alkaloid, absorption number is at least 2 times, and it is dry to be equivalent to radix dactylicapni medicinal material for the additional amount of cation exchange resin when adsorbing every time
0.5h is at least adsorbed in the 1/20 ~ 1/10 of product every time, and magnetic agitation absorption, stirring rate is 300 ~ 500rpm, after merging absorption
Cation exchange resin, after washing is filtered to remove surface impurity and be in neutrality washing efflux, by cation exchange resin
It is transferred in beaker, 10 ~ 30% aqueous sodium carbonate for being equivalent to 20 ~ 50 times of cation exchange resin dry weight amounts, ultrasound is added
It extracts 3 ~ 4 times, for the control of ultrasonic extraction temperature at 50 ~ 70 DEG C, supersonic frequency is 20 ~ 40kHz, and each ultrasonic time is no less than
40min merges ultrasonic extraction liquid, and filtrate is concentrated through reverse osmosis membrane after filtering, is cation exchange tree when being concentrated into medicine liquid volume
After 0.5 ~ 1 times of amount of rouge dry weight, stop concentration, after concentrate reinforces alkali adjusting pH to 10 ~ 11,0 DEG C of refrigeration at least 5h, centrifugation,
Discard supernatant liquid, centrifugation is washed to dry after neutrality, Biflorine crude product A is obtained, by opium alkali crude product A with being equivalent to opium
The chloroform stirring and dissolving at least 30min of 15 ~ 20 times of amounts of alkali crude product A weight, is then filtered, and filtrate is dry, obtains opium alkali crude product
B dissolves the double solvents of Biflorine crude product B chloroform and isopropanol, and the volume ratio of chloroform and isopropanol is 1:(1 ~ 3),
The additional amount of double solvents is equivalent to 4 ~ 5 times of amounts of Biflorine crude product B, after dissolution, filters, pure second is added dropwise in filtrate
Alcohol, stirring while adding, the additional amount of straight alcohol is equivalent to 10 ~ 15 times of amounts of Biflorine crude product B, after being added dropwise, is put in 0 ~ 5
DEG C refrigerator cold-storage is stayed overnight, and next day takes out, and suction filtration precipitates crystal, and straight alcohol washes removal surface impurity, then dries, and obtains former opium
Alkali Protopine monomer, purity are not less than 80%.
Preferably, the grinding particle size of radix dactylicapni medicinal material dry product is 100 ~ 200 mesh.
Preferably, aqueous acid includes aqueous acetic acid.
Preferably, cation exchange resin is strongly acidic cation-exchange.
It is further preferred that strongly acidic cation-exchange includes 731,732, it is any one in D001, D002, D006
Kind.
Preferably, opium alkali crude product B is using ultrasonic dissolution in the dissolving method of double solvents, and ultrasonic dissolution temperature is higher than
60 DEG C, supersonic frequency is 5 ~ 10kHz.
Preferably, highly basic includes NaOH or KOH.
Preferably, by purity not less than 80% Biflorine Protopine monomer with being equivalent to Biflorine Protopine
After the ethyl alcohol infiltration of 1 ~ 2 times of amount of monomer weight, ODS adsorbent is added and mixes sample, the additional amount of ODS adsorbent is equivalent to former opium
1 ~ 1.5 times of amount of alkali Protopine monomer crushes after being put in 40 ~ 50 DEG C of baking oven drying, obtains ODS and mix all product and fill column, column
Filler is blank ODS adsorbent, and the dress column amount of blank ODS adsorbent is equivalent to 2 ~ 4 times of amounts that ODS mixes all product, the diameter of pillar
Height is than being 1:(4 ~ 5), after filling column, utilize chloroform: isopropanol: methanol=1:(2 ~ 2.5): (1 ~ 1.5) elutes 5 ~ 8 column volumes, washes
After de- liquid is concentrated into 7 ~ 10 times of amounts of Biflorine Protopine monomer weight, knot is precipitated in -20 ~ -10 DEG C of 8 ~ 10h of refrigerator cold-storage
Crystalline substance, filtering, crystallizing and drying must refine Biflorine Protopine monomer, and purity is not less than 95%.
Radix dactylicapni Protopine Protopine monomer relieving cough and asthma preparation, analgesia preparation, anti-arrhythmia preparation or
Application in anti-tumor agent.
The beneficial effects of the present invention are:
1. technique of the invention is suitble to the Extraction and enrichment purifying of radix dactylicapni Protopine, and Biflorine purity is up to 80%
More than, further up to 95% or more after purification, the operating procedure of entire technique is simple and easy, and high income is at low cost.
2. present invention process process is stablized, the reagent largely used is safe and non-toxic, and the solvent toxicity that whole process uses is lower,
Environmentally friendly, non-environmental-pollution is suitble to high-volume industrial production.
3. the present invention for the first time recrystallizes Biflorine using double solvents, and using ODS filler to Biflorine
It is further refined, trace impurity ingredient capaurine, the isocorydine etc. in radix dactylicapni can be effectively removed, greatly improve original
Opium alkali purity, entire process operability is strong, and reproducibility is strong, is later radix dactylicapni Protopine large-scale industrial production
Technical parameter is provided.
Detailed description of the invention
Fig. 1 is the canonical plotting of Protopine of the present invention；
Fig. 2 is the chromatogram that Biflorine Protopine monomer is refined in the present invention.
Specific embodiment
The present invention will be further explained below.
Embodiment 1:
1. instrument and reagent: round-bottomed flask；Condenser pipe；Beaker；Suction funnel；(diameter height compares for 1:4), perseverance small-size glass chromatographic column
Warm magnetic stirring apparatus (DF-101S, Yuhua Instrument Co., Ltd., Gongyi City)；Assay balance (Mei Tele-support benefit)；Rotation
Evaporimeter (RE-52AA, Shanghai Yarong Biochemical Instrument Plant)；Ultrasound Instrument (DS-8510DT, the raw analysis limited public affairs of ultrasonic instrument in Shanghai
Department)；Digital display thermostat water bath (HH-4, Changzhou Guohua Electric Appliance Co., Ltd.)；Reverse osmosis membrane assembly and device (bw30-365, beauty
Tao Shi film company, state)；High performance liquid chromatograph (Shimadzu)；Refrigerator (BCD-206STPQ, Haier)；Methanol；Ethyl alcohol；Isopropanol；Three
Chloromethanes；Sodium carbonate；Acetic acid；Sodium hydroxide；Potassium hydroxide；Agents useful for same is that analysis is pure；731 cation exchange resins (on
Hai Kaiping resin Co., Ltd)；ODS filler (YMC company)；Biflorine standard items (are studied purchased from Chinese food drug assay
Institute).
2. chromatographic condition
Chromatographic column: Shimadzu VP-ODS (150 × 4.6 mm, 5 μm)；Mobile phase is that 0.6 % glacial acetic acid aqueous solution (contains 0.06
% triethylamine)-acetonitrile (81: 19)；Detection wavelength 280nm；Flow velocity: 1 mL/min；35 DEG C of column temperature.
3. the preparation of Biflorine reference substance solution: precision weighs 5 mg of reference substance Biflorine and sets 100 mL volumetric flasks
In, the imitative dissolution of chlorination is diluted to scale, shakes up to get wherein every mL 0.05 mg containing Biflorine.
4. the drafting of standard curve:
Linear relationship is investigated: precision draws Biflorine reference substance solution (0.05mg/mL) 5,10,15,20,25 μ L, by above-mentioned
Chromatographic condition measures peak area, using peak area Y as ordinate, with sample volume X(μ g) it is abscissa, regression analysis is carried out, must be returned
Return equation Y=1214.1X-6.697, R2=0.9997, as shown in Figure 1, showing that Biflorine linearly closes between 0.25 ~ 1.25 μ g
System is good.
5. the content measurement of radix dactylicapni medicinal material: taking radix dactylicapni medicinal material dry product powder (crossing 250 meshes) about 1g, precision claims
It is fixed, it is 1.0091g, sets in 50 mL triangular flask, add 9% aqueous acetic acid of 1 mL to infiltrate, add chloroform 20mL, seals
It closes, 2 h of ultrasound, filters, volatilize chloroform, residue adds methanol dissolution constant volume in 10mL volumetric flask, obtains radix dactylicapni medicinal material test sample
Solution.
5 μ L of radix dactylicapni medicinal material test solution is taken, high performance liquid chromatograph is injected, detection obtains in radix dactylicapni medicinal material dry product
The percentage composition of Biflorine is 0.1318%.
The Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer, includes the following steps: to take 1kg radix dactylicapni
Medicinal material Dactylicapnos scandens (D. Don) Hutch. dry product, is crushed to 100 mesh or so, is put in round-bottomed flask
In, 10L pure water is added, stirs and steeped overnight, next day discards maceration extract, 9% aqueous acetic acid of 8L, heat are added in the dregs of a decoction
Refluxing extraction 2 times, each extraction time is 1h, and Extracting temperature is 70 DEG C, merges acetic acid aqueous extract, is concentrated into extraction concentrate
Density when being 1.08 or so, stop concentration, 731 cationic exchange resin adsorption total alkaloids are added in filtrate in filtering, adsorb
Number is 2 times, and the additional amount of 731 cation exchange resins is 50g when absorption every time, adsorbs 0.5h every time, and magnetic agitation is adsorbed,
Stirring rate is 300rpm, and 731 cation exchange resins after merging absorption, washing is filtered to remove 731 cation exchange trees
Rouge surface impurity and making is washed after efflux is in neutrality, and 731 cation exchange resins are transferred in beaker, the 10% of 2L is added
Aqueous sodium carbonate, ultrasonic extraction 3 times, the control of ultrasonic extraction temperature is at 50 DEG C, supersonic frequency 20kHz, each ultrasonic time
For 40min, merging ultrasonic extraction liquid, filtrate is concentrated through reverse osmosis membrane after filtering, after being concentrated into medicine liquid volume is 50mL or so,
Stop concentration, after concentrate adds the adjusting of NaOH highly basic pH to 10,0 DEG C of refrigeration 5h, centrifugation discards supernatant liquid, centrifugation washing
It is dry after to neutrality, Biflorine crude product A is obtained, is weighed, weight 2.57g is molten with the stirring of 38mL chloroform by opium alkali crude product A
30min is solved, is then filtered, filtrate is dry, obtains opium alkali crude product B, weighs, and the weight of Biflorine crude product B is 2.04g, will be former
The dissolution of the double solvents of opium alkali crude product B chloroform and isopropanol, the additional amount of double solvents are 8 ~ 9mL, chloroform and isopropanol
Volume ratio be 1:1, after dissolution, filtering, opium alkali crude product B is the ultrasound using ultrasonic dissolution in the dissolving method of double solvents
Solution temperature is 65 DEG C, supersonic frequency 5kHz, straight alcohol is added dropwise in filtrate, stirring while adding, the additional amount of straight alcohol
For 10mL, after being added dropwise, it is put in 0 ~ 5 DEG C of refrigerator cold-storage and stays overnight, next day takes out, and suction filtration precipitates crystal, and straight alcohol washes removal
Then surface impurity is dried, Biflorine Protopine monomer 1.53g, purity 86.14% are obtained.It is 86.14% by purity
Biflorine Protopine monomer with 1.5mL ethyl alcohol infiltrate after, the ODS adsorbent that 1.5g is added mixes sample, is put in 40 after mixing sample
The drying of DEG C baking oven, crushes, obtains ODS and mix all product and fill column, and column packing is 6g blank ODS adsorbent, and it is 1 that the diameter height of pillar, which compares:
4, after filling column, utilize chloroform: isopropanol: methanol=1:2:1 elutes 5 column volumes, and eluent is concentrated into 10mL or so, in -20 DEG C
Crystallization, filtering is precipitated in refrigerator cold-storage 8h, and crystallizing and drying must refine Biflorine Protopine monomer 0.76g, as shown in Fig. 2,
Its purity is 98.64%, yield 57%.
Radix dactylicapni Protopine Protopine monomer relieving cough and asthma preparation, analgesia preparation, anti-arrhythmia preparation or
Application in anti-tumor agent.
Embodiment 2:
The Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer, includes the following steps: to take used in 1kg embodiment 1
Radix dactylicapni medicinal material dry product, crush, grinding particle size is 200 mesh or so, and smashed radix dactylicapni medicinal material is put in a round bottom flask, is added
Enter 20L pure water solution, stir and steeped overnight, next day discard maceration extract, 10% aqueous acetic acid of 13L is added in the dregs of a decoction,
Circumfluence distillation 5 times, each extraction time is 3h, and Extracting temperature is 80 DEG C, merges acetic acid aqueous extract, is concentrated into extraction concentration
When the density of liquid is 1.15 or so, stop concentration, filter, D001 cationic exchange resin adsorption total alkaloid is added in filtrate,
Adsorbing number is 3 times, and the additional amount of D001 cation exchange resin is 100g when absorption every time, adsorbs 1h, magnetic agitation every time
Absorption, stirring rate 500rpm, the D001 cation exchange resin after merging absorption, washing are filtered to remove D001 cation
Exchanger resin surface impurity and making is washed after efflux is in neutrality, and D001 cation exchange resin is transferred in beaker, is added
30% aqueous sodium carbonate of 15L, ultrasonic extraction 4 times, ultrasonic extraction temperature is controlled at 70 DEG C, supersonic frequency 40kHz, often
Secondary ultrasonic time is 60min, merges ultrasonic extraction liquid, filtrate is concentrated through reverse osmosis membrane after filtering, is when being concentrated into medicine liquid volume
After 300mL, stop concentration, after concentrate adds the adjusting of KOH highly basic pH to 11,0 DEG C of refrigeration 7h, centrifugation discards supernatant liquid, and centrifugation is heavy
Shallow lake is washed to drying after neutrality, obtains Biflorine crude product A, weighs, and the weight of Biflorine crude product A is 3.04g, and opium alkali is thick
Product A 60mL chloroform stirring and dissolving 70min, is then filtered, and filtrate is dry, obtains opium alkali crude product B, is weighed, Biflorine crude product B
Weight be 2.75g, by the double solvents of Biflorine crude product B chloroform and isopropanol dissolve, the volume of chloroform and isopropanol
Than for 1:3, the dosage of double solvents is 11 ~ 12mL, after dissolution, filtering, opium alkali crude product B is in the dissolving method of double solvents
Using ultrasonic dissolution, ultrasonic dissolution temperature is 80 DEG C, supersonic frequency 10kHz, and 40mL straight alcohol, Bian Jia is added dropwise in filtrate
Side stirring after being added dropwise, is put in 5 DEG C of refrigerator cold-storages and stays overnight, and next day takes out, and suction filtration precipitates crystal, and straight alcohol washes removal table
Face impurity, is then dried, and obtains Biflorine Protopine monomer 1.64g, purity 80.37%.It is 80.37% former by purity
After opium alkali Protopine monomer is infiltrated with 3.5mL ethyl alcohol, the ODS adsorbent that 2.5g is added mixes sample, is then put in 50 DEG C of baking ovens
It after drying, crushes, obtains ODS and mix all product and fill column, column packing is 16g blank ODS adsorbent, and the diameter height of pillar compares for 1:5, dress
After column, utilize chloroform: isopropanol: methanol=1:2.5:1.5 elutes 8 column volumes, after eluent is concentrated into 16mL, in -10 DEG C
Crystallization, filtering is precipitated in refrigerator cold-storage 10h, and crystallizing and drying must refine Biflorine Protopine monomer 0.83g, and purity is
96.05%, yield 60%.
Radix dactylicapni Protopine Protopine monomer relieving cough and asthma preparation, analgesia preparation, anti-arrhythmia preparation or
Application in anti-tumor agent.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer, which comprises the steps of: take
Appropriate radix dactylicapni medicinal material dry product, crushes, is put in extractor, is added and is equivalent to 10 ~ 20 times of weight of radix dactylicapni medicinal material dry product amounts
Aqueous solution, is stirred and steeped overnight, next day discard maceration extract, is added in the dregs of a decoction and is equivalent to radix dactylicapni medicinal material dry product weight 8 ~ 13
9 ~ 10% aqueous acid of amount again, circumfluence distillation 2 ~ 5 times, each extraction time is 1 ~ 3h, and Extracting temperature is 70 ~ 80 DEG C, is closed
And acid water extracting liquid, be concentrated into and extract the density of concentrate when being 1.08 ~ 1.15, stop concentration, filtering, be added in filtrate sun from
Sub-exchange resin adsorbs total alkaloid, and absorption number is at least 2 times, and the additional amount of cation exchange resin is suitable when absorption every time
In the 1/20 ~ 1/10 of radix dactylicapni medicinal material dry product, every time at least adsorb 0.5h, magnetic agitation absorption, stirring rate be 300 ~
500rpm, the cation exchange resin after merging absorption, washing are filtered to remove surface impurity and be in neutrality washing efflux
Afterwards, cation exchange resin is transferred in beaker, is added and is equivalent to the 10 ~ 30% of 20 ~ 50 times of cation exchange resin dry weight amounts
Aqueous sodium carbonate, ultrasonic extraction 3 ~ 4 times, the control of ultrasonic extraction temperature is at 50 ~ 70 DEG C, and supersonic frequency is 20 ~ 40kHz, often
Secondary ultrasonic time is no less than 40min, merges ultrasonic extraction liquid, and filtrate is concentrated through reverse osmosis membrane after filtering, when being concentrated into medical fluid body
Product is to stop concentration after 0.5 ~ 1 times of cation exchange resin dry weight is measured, and concentrate reinforces alkali and adjusts pH to 10 ~ 11, and 0 DEG C cold
After hiding at least 5h, centrifugation discards supernatant liquid, and centrifugation is washed to drying after neutrality, Biflorine crude product A is obtained, by opium alkali
The crude product A chloroform stirring and dissolving at least 30min for 15 ~ 20 times of amounts for being equivalent to opium alkali crude product A weight, is then filtered, filtrate
It is dry, opium alkali crude product B is obtained, the double solvents of Biflorine crude product B chloroform and isopropanol is dissolved, chloroform and isopropanol
Volume ratio is 1:(1 ~ 3), the additional amount of double solvents is equivalent to 4 ~ 5 times of amounts of Biflorine crude product B, after dissolution, filtering, filtrate
In straight alcohol is added dropwise, stirring while adding, the additional amount of straight alcohol is equivalent to 10 ~ 15 times of Biflorine crude product B amounts, is added dropwise
After, it is put in 0 ~ 5 DEG C of refrigerator cold-storage and stays overnight, next day takes out, and suction filtration precipitates crystal, and straight alcohol washes removal surface impurity, so
After dry, obtain Biflorine Protopine monomer, purity is not less than 80%.
2. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In the grinding particle size of radix dactylicapni medicinal material dry product is 100 ~ 200 mesh.
3. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In aqueous acid includes aqueous acetic acid.
4. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In cation exchange resin is strongly acidic cation-exchange.
5. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 4, feature exist
In, strongly acidic cation-exchange include 731,732, any one in D001, D002, D006.
6. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In opium alkali crude product B is using ultrasonic dissolution in the dissolving method of double solvents, and ultrasonic dissolution temperature is higher than 60 DEG C, supersonic frequency
Rate is 5 ~ 10kHz.
7. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In highly basic includes NaOH or KOH.
8. the Extraction and enrichment technique of radix dactylicapni Protopine Protopine monomer according to claim 1, feature exist
In by the ethyl alcohol leaching of Biflorine Protopine monomer 1 ~ 2 times of amount for being equivalent to Biflorine Protopine monomer weight
After profit, ODS adsorbent is added and mixes sample, the additional amount of ODS adsorbent is equivalent to 1 ~ 1.5 times of Biflorine Protopine monomer
Amount crushes after being put in 40 ~ 50 DEG C of baking oven drying, obtains ODS and mix all product and fill column, and column packing is blank ODS adsorbent, blank
The dress column amount of ODS adsorbent is equivalent to 2 ~ 4 times of amounts that ODS mixes all product, and the diameter height of pillar compares for 1:(4 ~ 5), after filling column, utilize
Chloroform: isopropanol: methanol=1:(2 ~ 2.5): (1 ~ 1.5) elutes 5 ~ 8 column volumes, and eluent is concentrated into Biflorine
After 7 ~ 10 times of amounts of Protopine monomer weight, crystallization is precipitated in -20 ~ -10 DEG C of 8 ~ 10h of refrigerator cold-storage, is filtered, crystallizing and drying,
Biflorine Protopine monomer must be refined, purity is not less than 95%.
9. radix dactylicapni Protopine Protopine monomer described in any one is in relieving cough and asthma system according to claim 1 ~ 8
Application in agent, analgesia preparation, anti-arrhythmia preparation or anti-tumor agent.
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