CN107936036A - A kind of disodium cantharidinate and preparation method thereof - Google Patents
A kind of disodium cantharidinate and preparation method thereof Download PDFInfo
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- CN107936036A CN107936036A CN201711223696.4A CN201711223696A CN107936036A CN 107936036 A CN107936036 A CN 107936036A CN 201711223696 A CN201711223696 A CN 201711223696A CN 107936036 A CN107936036 A CN 107936036A
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- disodium cantharidinate
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/18—Bridged systems
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Abstract
The invention discloses a kind of disodium cantharidinate and preparation method thereof, including following component：Chinese blister beetle, hydrochloric acid, acetone, absolute ethyl alcohol, petroleum ether, sodium hydroxide and medical charcoal；This disodium cantharidinate and preparation method thereof, weigh Chinese blister beetle coarse powder medicinal material and put refluxing extraction during implosion guard dipping fills, collect extracting solution and discard smoke filtrate, wash and remove impurity, obtain cantharidin crude product, recrystallize again plus after acetone solution, fling to acetone to crystallize separate out, filter, both cantharidin fine work is obtained, slowly instill sodium hydroxide solution, after complete reaction, add medical charcoal aqueous solution, filter while hot, up to disodium cantharidinate solution, processing is dried again, disodium cantharidinate fine powder purity made of reality is high, the effect for being dissolved in water is more outstanding, it is allowed to resource utilization higher in use, biological absorption also goes up therewith, preparation method selected material, actual production capacity protrudes, meet to maximize the finished product rate of recovery while equipment production requirement.
Description
Technical field
The present invention relates to pharmaceutical technology field, more particularly to a kind of disodium cantharidinate and preparation method thereof.
Background technology
Chinese blister beetle alias spot oyster, piebald hair, tabby, Yuan are blue or green, spend shell worm, Zhang Wa, soya bean worm etc., are commonly called as SPANISH FLY, spot
Chinese blister beetle is in oval, and long 1.5~2.5cm, wide 0.5~1cm, head and mouthpart downward vertically, there is larger compound eye and each 1 pair of feeler,
Feeler has come off more, and back tool keratin elytrum 1 is right, and black, having below the band wing of 3 yellow or brown has tan film shape
Transparent interior wing 2, thorax abdomen corvinus, chest have 3 pairs of foot, there is special foul smell, and Chinese blister beetle has very strong renal toxicity, belongs to severe toxicity
Article, can secrete the liquid for being referred to as cantharidin, for defending enemy, since ancient Greek's period, just have and use this liquid
As the record of aphrodisiac, Chinese blister beetle is the traditional cancer therapy drug in China, is mainly used for liver cancer, lung cancer, the carcinoma of the rectum, malignant lymphatic
The treatment of the malignant tumours such as knurl, cervical carcinoma, nasopharyngeal carcinoma, cutaneum carcinoma, myeloma, leukaemia, clinically there is good effect, mesh
Preceding in the market has the products such as cantharides capsule, ad pro injection, since the elimination of cantharidin in vivo is very fast, during clinical application
The peak valley fluctuation of blood concentration is easily caused, and it with stronger irritation, solubility in water is relatively low, oral bio profit
Expenditure is low, and existing preparation can not effectively overcome this defect, therefore selects more suitably preparation to improve the utilization rate of medicine,
The blood concentration of cantharidin held stationary in vivo is controlled, toxic side effect is reduced to improve curative effect, mitigates irritation on mucous membrane, become
For the task of top priority, cantharidin is to extract to be isolated from cantharis animal body, then by chemical synthesis into sodium salt
Obtain disodium cantharidinate raw material.
The content of the invention
Solve the problems, such as that existing utilization ratio of drug is low for this, cover certain side effect, it is an object of the invention to carry
For a kind of disodium cantharidinate and preparation method thereof, which possesses the fundamental characteristics that solubility is high, utilization rate is high, most prominent
It is that can preserve 2 years at normal temperatures without rotten tendency occurs, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical solution：A kind of disodium cantharidinate, including following component：Chinese blister beetle,
Hydrochloric acid, acetone, absolute ethyl alcohol, petroleum ether, sodium hydroxide and medical charcoal, and matched successively by following parts by weight：Chinese blister beetle 20Kg,
Hydrochloric acid 5500ml, 190,000 ml of acetone, 5000ml, 30-60 DEG C of petroleum ether 5000ml of absolute ethyl alcohol, appropriate sodium hydroxide and appropriate medicine
Use charcoal.
Preferably, Chinese blister beetle is coarse powder, and the substance withdrawl syndrome of sodium hydroxide solution is 20% (g/ml).
Another technical problem to be solved by the present invention is that providing a kind of preparation method of disodium cantharidinate, include the following steps：
S1：Cantharidin is extracted, weighs Chinese blister beetle coarse powder medicinal material 20Kg, puts during implosion guard dipping fills refluxing extraction three times, the
20% hydrochloric acid 200ml once is added by per kilogram medicinal material, when acidification 1 is small, then 3 times is added by per kilogram medicinal material and measures acetone,
70 DEG C of heating water baths, when refluxing extraction 3 is small, collect extracting solution, repetitive operation is extracted 3 times, merges extracting solution, concentration and recovery third
Ketone, concentrate filter while hot, discard smoke filtrate, residue 30-60 DEG C of petroleum ether and absolute ethyl alcohol proportionally 1:1 is washed
Wash and remove impurity, obtain cantharidin crude product；
S2：Disodium cantharidinate synthesis, refined, cantharidin crude product recrystallizes after adding acetone solution, flings to acetone and separates out to crystallizing,
Filter, both obtain cantharidin fine work, claim cantharidin fine work to be placed in reaction kettle, add acetone, after heating water bath reflux makes dissolving, delay
20% (g/ml) sodium hydroxide solution of slow dropwise addition, it is stirring while adding, after sodium hydroxide solution is added completely into, continue stirring reaction
Two hours, after complete reaction, the medical charcoal aqueous solution of solution total amount 3 ‰~5 ‰ is added, continue heating water bath and flow back 30 points
Clock, filters while hot, obtains water white transparency filtrate, i.e. disodium cantharidinate solution, filtrate water-bath is concentrated to dryness, up to white powder Chinese blister beetle
Sour sodium；
S3：The drying of disodium cantharidinate, extraction white powder disodium cantharidinate, which is placed in drying box, to be dried；
S4：Sampling amount and the amount of keeping sample, according to the demand of inspection, the sampling amount of intermediate products, that is, cantharidin is 1.5g, and finished product is
The sampling amount of disodium cantharidinate is 1.5g, and the amount of keeping sample of disodium cantharidinate finished product is 2.5g；
S5：The packing of disodium cantharidinate：Use packing specification for 10g/ bottles oral stable medicinal polythene bottle with high density into
Row packing.
Preferably, according in S2, the yield of cantharidin is the 0.7%~0.9% of medicinal material inventory, the addition of acetone according to
The amount that 1g cantharidins are dissolved in 40ml acetone is quantitatively added, and the temperature setting of heating water bath is at 68 DEG C to 72 DEG C.
Preferably, according in S3, the yield of disodium cantharidinate is the 0.9%~1.2% of medicinal material inventory, environment in drying box
68 DEG C to 72 DEG C should be arranged to, white powder disodium cantharidinate moisture is less than 5.0% after the completion of drying.
Preferably, according to dried disodium cantharidinate in S5, is taken in packing room, by 10g/ bottles of packing specification electronic balances
Weighing carries out weighing packing, is numbered on every bottle of label, the particular number of indicating less than 10g, and carries out weighing record, and has
Review.
Compared with prior art, the beneficial effects of the invention are as follows：This disodium cantharidinate and preparation method thereof, with Chinese blister beetle, hydrochloric acid,
Acetone, absolute ethyl alcohol etc. are used as raw material, multiple steps such as are extracted, synthesized, filtered, refined, dried, dispensed successively, actual
Manufactured disodium cantharidinate fine powder purity is high, is dissolved in that the effect of water is more outstanding, is allowed to resource utilization in use more
Height, biological absorption also go up therewith, preparation method selected material, and actual production capacity protrudes, while meeting equipment production requirement
Maximize the finished product rate of recovery.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention.
Embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment, belongs to the scope of protection of the invention.
Referring to Fig. 1, a kind of disodium cantharidinate, including following component：Chinese blister beetle, hydrochloric acid, acetone, absolute ethyl alcohol, petroleum ether, hydrogen
Sodium oxide molybdena and medical charcoal, and matched successively by following parts by weight：Chinese blister beetle 20Kg, hydrochloric acid 5500ml, 190,000 ml of acetone, anhydrous second
5000ml, 30-60 DEG C of petroleum ether 5000ml of alcohol, appropriate sodium hydroxide and appropriate medical charcoal, wherein, Chinese blister beetle is coarse powder, hydroxide
The substance withdrawl syndrome of sodium solution is 20% (g/ml), and Chinese blister beetle authentication process is as follows, takes this product powder 2g, and chlorination imitates 20ml, is surpassed
Filtrate is simultaneously evaporated by sonication 15min, filtration treatment, and residue 30~60 DEG C of petroleum ethers 2 times, each 5ml, carefully inclines
Supernatant, residue chlorination, which imitates 1ml, makes dissolving, as test solution, separately takes cantharidin reference substance, chlorination is copied into every 1ml and contained
The solution of 5mg, as reference substance solution, is tested according to thin-layered chromatography, draw each 5 μ l of above two solution, put respectively in
On same silica gel g thin-layer plate, chloroform-acetone, as solvent, is unfolded and takes out to dry, spray with 0.1% according to 49 to 1 ratio
Bromocresol green ethanol solution, it is clear to be heated to spot development, in test sample chromatography, on position corresponding with reference substance chromatography,
The spot of aobvious same color, using its content of high effective liquid chromatography for measuring, using octadecylsilane chemically bonded silica as filler,
With methanol-water (23:77) it is mobile phase, Detection wavelength 230nm, number of theoretical plate calculates not lower than 3000 by cantharidin peak,
Take cantharidin reference substance appropriate, it is accurately weighed, add methanol that the solution of every 1ml 1mg containing cantharidin is made, you can it is molten to complete reference substance
The preparation of liquid, then this product coarse powder about 1g is taken, it is accurately weighed, put in conical flask with cover, chlorination imitates supersound process (power 400W, frequency
Rate 40kHz) 2 times, each 30ml, 15 minutes, merge chloroform solution, filtering, with a small amount of chloroform gradation washing container, washing lotion and filtrate
Merging, for recycling design to dry, residue adds methanol to make dissolving, and is transferred in 10ml measuring bottles, adds methanol to shake up, filter to scale,
Take subsequent filtrate, you can the preparation of test solution, then accurate absorption reference substance solution and each 10 μ l of test solution respectively are completed,
Inject liquid chromatograph, measure, up to structure, this product (C containing cantharidin10H12O4) 0.35% must not be less than.
Another technical problem to be solved by the present invention is that providing a kind of preparation method of disodium cantharidinate, include the following steps：
The first step：Cantharidin is extracted, weighs Chinese blister beetle coarse powder medicinal material 20Kg, quantitative throwing is carried out according to existing production equipment
Put, if inventory very little, extracts the amount of cantharidin with regard to seldom, loss is just bigger in process of production, and the yield of finished product is just
It can reduce, if exceeding 20Kg, can cannot meet production requirement because the volume of equipment is small, selected material, meets that equipment produces
It is required that while maximize the finished product rate of recovery, Chinese blister beetle coarse powder medicinal material is placed in during implosion guard dipping fills refluxing extraction three times, the
20% hydrochloric acid 200ml once is added by per kilogram medicinal material, when acidification 1 is small, then 3 times is added by per kilogram medicinal material and measures acetone,
70 DEG C of heating water baths, when refluxing extraction 3 is small, collect extracting solution, repetitive operation is extracted 3 times, merges extracting solution, concentration and recovery third
Ketone, concentrate filter while hot, discard smoke filtrate, residue 30-60 DEG C of petroleum ether and absolute ethyl alcohol proportionally 1:1 is washed
Wash and remove impurity, obtain cantharidin crude product；
Second step：Disodium cantharidinate synthesis, refined, cantharidin crude product recrystallizes after adding acetone solution, the addition of acetone according to
The amount that 1g cantharidins are dissolved in 40ml acetone is quantitatively added, and is flung to acetone to precipitation is crystallized, is filtered, newly into acetone and recycling third
The ratio of ketone is 1:1, it is ensured that quantitative accurate, both obtains cantharidin fine work, claims cantharidin fine work to be placed in reaction kettle, adds acetone,
After heating water bath reflux makes dissolving, 20% (g/ml) sodium hydroxide solution is slowly added dropwise, it is stirring while adding, treat sodium hydroxide solution
After being added completely into, continue stirring reaction two hours, after complete reaction, the medical charcoal for adding solution total amount 3 ‰~5 ‰ is water-soluble
Liquid, continues heating water bath and flows back 30 minutes, the temperature setting of heating water bath filters at 68 DEG C to 72 DEG C, obtain water white transparency while hot
Filtrate, i.e. disodium cantharidinate solution, filtrate water-bath is concentrated to dryness, and up to white powder disodium cantharidinate, the yield of cantharidin is medicine
The 0.7%~0.9% of material inventory, reaction equation are：C10H12O4+ 2NaOH=C10H12O5Na2+H2O,
Computational methods are as follows,
Wherein：196.2 be the molecular weight of cantharidin；
40 be the molecular weight of sodium hydroxide；
X by palpus sodium hydroxide amount (g)；
A is the amount (g) of cantharidin；
2 be the molar ratio of sodium hydroxide and cantharidin；
3rd step：The drying of disodium cantharidinate, extraction white powder disodium cantharidinate, which is placed in drying box, to be dried, cantharidic acid
The yield of sodium is the 0.9%~1.2% of medicinal material inventory, and environment should be arranged to 68 DEG C to 72 DEG C, after the completion of dry in drying box
White powder disodium cantharidinate moisture is less than 5.0%；
4th step：Sampling amount and the amount of keeping sample, according to the demand of inspection, the sampling amount of intermediate products, that is, cantharidin is 1.5g, into
The sampling amount of product, that is, disodium cantharidinate is 1.5g, and the amount of keeping sample of disodium cantharidinate finished product is 2.5g, and cantharidin authentication process is as follows, takes this
Product fine powder is appropriate (being approximately equivalent to cantharidin 5mg), and after chlorination imitates 10ml dippings, filtering, takes filtrate to add dilute hydrochloric acid to acidity, Yu Shui
Heating evaporation adds sulfuric acid 2~3 to drip to there is crystallization to separate out in bath, and small fire heating, that is, bubble occur, stop heating immediately, and be added dropwise
Paradime thylaminobenzaldehyde sulfuric acid solution 1~2 drips, the i.e. aobvious lilac red of solution, weighs that hexadecane is appropriate, and chlorination is copied into every
Solution of the 1ml containing 0.5mg, as inner mark solution, then takes that about 10mg cantharidin reference substances are appropriate, and accurately weighed, chloroform is settled to
50ml；Precision is drawn in above-mentioned solution 5ml to 10ml measuring bottles, then accurate plus inner mark solution 2ml, chloroform are diluted to scale, are
Solution per 1ml 0.1mg containing cantharidin and hexadecane 0.1mg, as reference substance solution, precision weighs this product about 10mg, extremely
In 25ml volumetric flasks, chlorination, which is imitated, dissolves and is diluted to scale；Filtering, precision measure filtrate 1ml, then accurate plus inner mark solution 2ml,
Mix, be transferred in 10ml measuring bottles, be diluted to scale with chloroform, shake up, be test solution, draw reference substance solution respectively
With each 2 μ l of test solution, gas chromatograph is injected, measure, calculates content, up to as a result, this product is calculated by dry product, containing spot
Chinese blister beetle element must not be less than 96.0%；
5th step：The packing of disodium cantharidinate：Packing specification is used as the medicinal high density polyethylene (HDPE) of 10g/ bottles of oral administration solid
Bottle is dispensed, and takes dried disodium cantharidinate to be weighed in packing room by 10g/ bottles of packing specifications with electronic balance weighing
Packing, is numbered, the particular number of indicating less than 10g on every bottle of label, and carries out weighing record, and has review, into quality
It is as follows to measure the method for inspection：Take disodium cantharidinate fine powder appropriate, be approximately equivalent to disodium cantharidinate 10mg, after adding water 20ml to impregnate, filtering, takes
Filtrate is tested by the following method：Barium chloride test solution is added, that is, produces white precipitate；This product is taken after loss on drying, in 105 DEG C of dryings
To constant weight, less loss weight must not exceed 5.0%, is measured according still further to gas chromatography, be fixation with methyl silica gel (SE-30)
Liquid, coating concentration 10%；Column temperature is 180 DEG C；Number of theoretical plate is calculated by cantharidin peak, should be not less than 3000, be weighed hexadecane
In right amount, chloroformic solutions of every 1ml containing 2mg is made, as inner mark solution, then takes cantharidin reference substance appropriate, it is accurately weighed, add interior
Mark that solution is appropriate, and chlorination copies into the solution of every 1ml 0.3mg containing cantharidin and hexadecane 0.2mg, as reference substance solution,
Precision weighs this product 6mg and puts in conical flask, adds 1mol/L sulfuric acid liquid 20ml, and 65 DEG C of water-baths flow back 30 minutes, moved after slightly cold in point
In liquid funnel, with chloroform 25,15,10ml extractions three times, 10 minutes every time；Combining extraction liquid, 70 DEG C of water-baths fling to chloroform to about
5ml, is transferred in 10ml measuring bottles, and precision plus internal standard solution 1ml, are diluted to scale with chloroform, shake up, and is test solution, point
Not Xi Qu reference substance solution and each 2 μ l of test solution, inject gas chromatograph, record chromatography, by peak area based on internal standard method
Content is calculated, multiplied by with 1.316, up to measurement result, this product is calculated by dry product, containing C10H12Na2O595.0% must not be less than.
In conclusion disodium cantharidinate proposed by the present invention and preparation method thereof, with Chinese blister beetle, hydrochloric acid, acetone, absolute ethyl alcohol etc.
As raw material, multiple steps such as extracted, synthesized, being filtered, being refined, being dried, being dispensed successively, weigh Chinese blister beetle coarse powder medicinal material put it is anti-
Refluxing extraction during quick-fried glass-impregnated fills, collects extracting solution and discards smoke filtrate, wash and remove impurity, obtains cantharidin crude product, then add
Recrystallized after acetone solution, fling to acetone to precipitation is crystallized, filter, both obtain cantharidin fine work, slowly instill sodium hydroxide solution,
After complete reaction, medical charcoal aqueous solution is added, filters while hot, up to disodium cantharidinate solution, then processing is dried, actual system
Into disodium cantharidinate fine powder purity it is high, be dissolved in that the effect of water is more outstanding, be allowed to resource utilization higher in use,
Biological absorption also goes up therewith, preparation method selected material, and actual production capacity protrudes, and meets maximum while equipment production requirement
The chemical conversion product rate of recovery.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of disodium cantharidinate, it is characterised in that including following component：Chinese blister beetle, hydrochloric acid, acetone, absolute ethyl alcohol, petroleum ether, hydrogen
Sodium oxide molybdena and medical charcoal, and matched successively by following parts by weight：Chinese blister beetle 20Kg, hydrochloric acid 5500ml, 190,000 ml of acetone, anhydrous second
5000ml, 30-60 DEG C of petroleum ether 5000ml of alcohol, appropriate sodium hydroxide and appropriate medical charcoal.
A kind of 2. disodium cantharidinate as claimed in claim 1, it is characterised in that：Chinese blister beetle is coarse powder, the material of sodium hydroxide solution
Amount concentration be 20% (g/ml).
3. a kind of preparation method of disodium cantharidinate as claimed in claim 1, it is characterised in that include the following steps：
S1：Extract cantharidin, weigh Chinese blister beetle coarse powder medicinal material 20Kg, put implosion guard dipping fill in refluxing extraction three times, for the first time
By per kilogram medicinal material add 20% hydrochloric acid 200ml, when acidification 1 is small, then by per kilogram medicinal material add 3 times amount acetone, 70 DEG C
Heating water bath, when refluxing extraction 3 is small, collects extracting solution, repetitive operation is extracted 3 times, merges extracting solution, and concentration and recovery acetone is dense
Contracting liquid filters while hot, discards smoke filtrate, residue 30-60 DEG C of petroleum ether and absolute ethyl alcohol proportionally 1:1 is washed simultaneously
Impurity is removed, obtains cantharidin crude product；
S2：Disodium cantharidinate synthesis, refine, and cantharidin crude product recrystallizes after adding acetone solution, flings to acetone to precipitation is crystallized, takes out
Filter, both obtains cantharidin fine work, claims cantharidin fine work to be placed in reaction kettle, adds acetone, after heating water bath reflux makes dissolving, slowly
20% (g/ml) sodium hydroxide solution is added dropwise, it is stirring while adding, after sodium hydroxide solution is added completely into, continue stirring reaction two
Hour, after complete reaction, the medical charcoal aqueous solution of solution total amount 3 ‰~5 ‰ is added, continue heating water bath and flow back 30 points
Clock, filters while hot, obtains water white transparency filtrate, i.e. disodium cantharidinate solution, filtrate water-bath is concentrated to dryness, up to white powder Chinese blister beetle
Sour sodium；
S3：The drying of disodium cantharidinate, extraction white powder disodium cantharidinate, which is placed in drying box, to be dried；
S4：Sampling amount and the amount of keeping sample, according to the demand of inspection, the sampling amount of intermediate products, that is, cantharidin is 1.5g, finished product, that is, Chinese blister beetle
The sampling amount of sour sodium is 1.5g, and the amount of keeping sample of disodium cantharidinate finished product is 2.5g；
S5：The packing of disodium cantharidinate：Packing specification is used to be divided for 10g/ bottles of oral stable medicinal polythene bottle with high density
Dress.
A kind of 4. preparation method of disodium cantharidinate as claimed in claim 3, it is characterised in that according in S2, the receipts of cantharidin
Rate is the 0.7%~0.9% of medicinal material inventory, and the amount that the addition of acetone is dissolved in 40ml acetone according to 1g cantharidins is quantitatively added
Put, the temperature setting of heating water bath is at 68 DEG C to 72 DEG C.
A kind of 5. preparation method of disodium cantharidinate as claimed in claim 3, it is characterised in that according in S3, disodium cantharidinate
Yield is the 0.9%~1.2% of medicinal material inventory, and environment should be arranged to 68 DEG C to 72 DEG C in drying box, white after the completion of drying
Powder disodium cantharidinate moisture is less than 5.0%.
6. a kind of preparation method of disodium cantharidinate as claimed in claim 3, it is characterised in that dried according in S5, taking
Disodium cantharidinate carries out weighing packing with electronic balance weighing by 10g/ bottles of packing specifications, is compiled on every bottle of label in packing room
Number, the particular number of indicating less than 10g, and weighing record is carried out, and have review.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711223696.4A CN107936036A (en) | 2017-11-29 | 2017-11-29 | A kind of disodium cantharidinate and preparation method thereof |
| CN201810344550.3A CN108250210A (en) | 2017-11-29 | 2018-04-17 | A kind of disodium cantharidinate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711223696.4A CN107936036A (en) | 2017-11-29 | 2017-11-29 | A kind of disodium cantharidinate and preparation method thereof |
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| CN107936036A true CN107936036A (en) | 2018-04-20 |
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| CN201711223696.4A Withdrawn CN107936036A (en) | 2017-11-29 | 2017-11-29 | A kind of disodium cantharidinate and preparation method thereof |
| CN201810344550.3A Pending CN108250210A (en) | 2017-11-29 | 2018-04-17 | A kind of disodium cantharidinate and preparation method thereof |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810344550.3A Pending CN108250210A (en) | 2017-11-29 | 2018-04-17 | A kind of disodium cantharidinate and preparation method thereof |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1166669C (en) * | 2002-03-20 | 2004-09-15 | 贵州君之堂制药有限公司 | Prepn process of sodium cantharidinate |
| CN100545164C (en) * | 2007-02-13 | 2009-09-30 | 北京世纪博康医药科技有限公司 | The preparation technology of disodium cantharidinate |
| CN102146086B (en) * | 2011-04-12 | 2012-03-07 | 贵州金桥药业有限公司 | Preparation method of sodium cantharidate |
| CN102276619A (en) * | 2011-06-21 | 2011-12-14 | 贵州金桥药业有限公司 | Method for preparing sodium canthanridate |
-
2017
- 2017-11-29 CN CN201711223696.4A patent/CN107936036A/en not_active Withdrawn
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| CN108250210A (en) | 2018-07-06 |
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