CN1076111A - Cantharidate anti-virus formulation and preparation thereof - Google Patents
Cantharidate anti-virus formulation and preparation thereof Download PDFInfo
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- CN1076111A CN1076111A CN 92106087 CN92106087A CN1076111A CN 1076111 A CN1076111 A CN 1076111A CN 92106087 CN92106087 CN 92106087 CN 92106087 A CN92106087 A CN 92106087A CN 1076111 A CN1076111 A CN 1076111A
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Abstract
A kind of anti-virus formulation that contains LITHIUM CANTHARIDATE, potassium, magnesium, calcium, copper, zinc, cobalt or germanium salt, the content of its cantharidate is 0.00001～1%.Said preparation is produced cantharidin and hydroxide that contains above-mentioned metallic element or oxide reaction.A large amount of clinical case histories show that these contain the preparation of cantharidate, to specific therapeutical effect of viral infection such as viral hepatitis, enteritis, tracheitis, condyloma acuminatum, flu, pink eye disease.In addition, the antivirus test that utilizes cell culture technology to carry out shows that cantharidate has direct deactivation to HIV (human immunodeficiency virus).Cantharidate preparation of the present invention is used for the prevention of human body, animal, the multiple virosis of plant, the sterilization for the treatment of and being used for virus.
Description
The invention provides a kind of anti-virus formulation that contains cantharidate and preparation method thereof, be the feedstock production cantharidate specifically by extracting cantharidin in the insect bodies such as Mylabris or adopting synthetic cantharidin, again the gained salt is prepared into various medicaments, this medicament is applicable to as people, animal, giving of the multiple virosis of plant to be prevented and healing potion and medicine ' Bingduxiao ' toxic agent.
Cantharidin is by what extract in the polypides such as insecticide Mylabris the hypertoxicity material to be arranged.Cantharis medically has the record of antitumor action very early as medicine in China.External classic Mylabris plaster is to be aided with Cera Flava, Colophonium, Adeps Bovis seu Bubali, the made vesicatory of Lignum Pini Nodi wet goods by powder of cantharide, powder of cantharide accounts for 25% in this cream, do not have through Calculation of Solubility and experimental observation cantharidin major part in system cream process dissolved, so this classic dermerethistica manufactured goods that are powder of cantharide.In recent years, found particularly that cantharidin can be used as after the anticarcinogen, the pharmacology of cantharidin and the research of using on clinical medicine had been developed by leaps and bounds.The method that at present prepares cantharidin and adopted is to utilize organic solvent, for example extracting from powder of cantharide such as acetone, chloroform.Increase yield for impelling cantharidate to change into cantharidin, so usually before, all be to handle powder of cantharide with concentrated hydrochloric acid with organic solvent extracting cantharidin.Gained cantharidin refabrication after purifying becomes medicament, just as, cantharidin sheet (Shanghai Q/WS-1-566-80) and cantharidin injection (Shanghai Q/WS-1-567-80).
In recent years find again medically that cantharidin is a kind of antiviral antibiotic, but cantharidin is also not obvious in the common non-fat-soluble cantharidin preparation effect of the intravital this antibiosis drug effect of humans and animals, and fat-soluble cantharidin demonstrates good effect (Nature Journal was rolled up 458 pages of 6 phases in 1980 3).Particularly, utilize fat-soluble cantharidin prepared preparation can play specific effect to the treatment of viral infection such as viral hepatitis, condyloma acuminatum.Inventor of the present invention once proposed a kind ofly to prepare the method for the fat-soluble intermediate preparation of cantharidin and utilize the base stock of prepared this intermediate preparation as active ingredient, the variant adjuvant of compatibility, be prepared into the technology of a series of antiviral antibiotic preparation, and applied for patent (application number: CN, No. 90106365).Show this class medicine through clinical trial, to viral infection such as viral hepatitis, condyloma acuminatum, specific therapeutical effect, with the antivirus test that cell culture technology carries out, this product has direct deactivation to HIV (human immunodeficiency virus).The following step is mainly adopted in the preparation of its fat-soluble cantharidin preparation of this technology:
1, at first use organic solvent, for example dipping powders of cantharide such as acetone, chloroform, dichloromethane, chloroform arrive organic facies with the composition extracting of Oleum Mylabris in the Mylabris and cantharidin;
2, through the dry button of the powder of cantharide of organic solvent extracting, reuse concentrated hydrochloric acid acetone soln floods, and concentrated hydrochloric acid can change into cantharidin with cantharidate, and acetone can dissolve cantharidin into organic facies;
3, cantharidin and Oleum Mylabris in above-mentioned 1 the organic facies are isolated from this organic facies after, add petroleum ether, the Oleum Mylabris extracting is gone out, and cantharidin is separated with Oleum Mylabris, cantharidin that obtains and above-mentioned 2 isolating cantharidin merging;
4, in refining oils and fats, fatty acid or aliphatic alcohol equal solvent by being metered into cantharidin, can add a certain amount of Oleum Mylabris again under 80～210 ℃ of temperature for increasing the dissolubility of cantharidin in solvent, normal pressure stirs heating down, makes fat-soluble cantharidin intermediate preparation.
The intermediate preparation of said process preparation adds other adjuvant by a certain percentage and can prepare the various medicaments that contain fat-soluble cantharidin.Utilize in the prepared various medicaments of fat-soluble cantharidin, the content of its cantharidin accounts for 0.00005～0.05% of medicament weight.But, the above-mentioned this medicine that contains cantharidia liposoluble pharmaceutics, its processing technique is more numerous, and prepared medicine cost of goods manufactured is also higher, and the fat-soluble preparation application process that has is easy inadequately, and the scope of application is subjected to fat-soluble restriction.In addition, contain cantharidin in polypides such as insecticide Mylabris, also contain MAGNESIUM CANTHARIDATE, POTASSIUM CANTHARIDATE, therefore, utilization Mylabris polypide is as oral medicine in Chinese medicine, and its drug effect also comprises the effect of cantharidate.Cantharidate is more soluble in water, but directly extract and make pure product cantharidate from the Mylabris polypide, various salts separate difficult, the method for purification complexity, yield is low, is far from easy, the saving, easily capable, suitable of method that first purification cantharidin is made pure product cantharidate then.Contain MAGNESIUM CANTHARIDATE, POTASSIUM CANTHARIDATE in the natural polypide, illustrate that cantharidate brings into play its of antibiosis in the Mylabris polypide biology, with cantharidin its advantage is arranged respectively, so cantharidate also is the antiviral drugs that its speciality is arranged compared with cantharidin.
The purpose of this invention is to provide a kind of anti-virus formulation (medicament) that contains cantharidate, the preparation process of this preparation is simple, medicament is easy to use, and viral disease had wide spectrum ground antivirus action, cantharidate not only has the specific antiviral therapy effect similar to fat-soluble cantharidin medicament to human body, and the preparation made of cantharidate is more suitable for being used for that giving of animal, the viroses of plant is anti-, treatment and use as the various disinfectants of kill virus.
Cantharidate anti-virus formulation provided by the present invention is meant and contains cantharidate and other adjuvant prepared preparation that LITHIUM CANTHARIDATE, potassium, magnesium, calcium, copper, zinc, cobalt or germanium salt are main component that the content of cantharidate (weight) is 0.00001～1% in its preparation.Cantharidate and medicaments preparation method thereof are mainly by following three steps:
1, the technology that once provided by the present inventor (application number CN, 90106365) or adopt other technology from polypides such as insecticide Mylabris, to extract the higher cantharidin of purity, or use the pure product cantharidin that synthetic method is made;
2, the cantharidin of above-mentioned 1 gained and the hydroxide or the oxide reaction of containing metal lithium, potassium, magnesium, calcium, copper, zinc, cobalt or germanium are made cantharidate;
3, above-mentioned 2 cantharidates that prepare are added adjuvant by a certain percentage and be prepared into the medicine system that contains cantharidate weight 0.00001～1%.
In above-mentioned preparation process 2, for making cantharidin energy abundant and metal hydroxides or reactive metal oxide, need control to participate in the equivalent of reactant, draft and drop into reactant by the chemical reaction equivalent, in order to make cantharidate be easy to generation, separation and purification, need to select suitable solvent, the present invention makees solvent at the preparation process of cantharidate water commonly used, also uses some mixed solution (for example: water and acetone, water and ethanol).When water is cooked the solvent of cantharidate preparation process, when being reactant with the hydroxide of the lithium metal, the potassium that are dissolved in or are slightly soluble in water, calcium or oxide and zinc hydroxide, the input amount of cantharidin should surpass the chemical reaction equivalent, make the hydroxide or the oxide complete reaction of participating in reaction, leach after the excessive cantharidin reaction, can participate in reaction again.When water is cooked the solvent of cantharidate preparation process, when being reactant with the hydroxide of water-fast magnesium metal, copper, cobalt or germanium or oxide and zinc oxide, the input amount of cantharidin should be less than or equal to the chemical equivalent value, make cantharidin energy complete reaction, after treating the cantharidin complete reaction, will not have the hydroxide or the oxide of reaction to leach.Be accelerated reaction simultaneously, the neutralization reaction of cantharidin and hydroxide or oxide can be carried out under heating, and preferable reaction temperature is 50～120 ℃, reacts when application is higher than the solvent boiling point temperature, needs airtight pressurization, is compressive reaction.
In above-mentioned cantharidate preparation process, in order to prevent that airborne carbonic acid gas from participating in course of reaction and generating carbonate, and influence the purity of cantharidate, in cantharidin and metal-oxide or the hydroxide course of reaction, to use the inaccessiable equipment of air, and earlier with nitrogen or do not contain other gases or the steam of carbonic acid gas, with containing the air emptying of carbonic acid gas in the reactor, then in the preparation of avoiding carrying out under the condition of carbonic acid gas cantharidate.When using more metal-oxide of its carbonate meltage in solvent and hydroxide, more need strict the execution to prevent that carbonic acid gas from entering the preparation method of chemical reaction as reactant.
Below by embodiment to further detailed being illustrated of preparation method of the present invention.
Example 1, the preparation of POTASSIUM CANTHARIDATE
By the method for aforementioned prior art (CN90106365 number), by extracting the cantharidin crystallization in the Mylabris polypide.In the inaccessiable reactor of air, drop into pure product cantharidin 10g, add 800 ml deionized water, add 40 milliliters of pure product 10% potassium hydroxide aqueous solutions, get rid of CO 2 aerated air, carry out neutralization reaction, constantly stir in the course of reaction at 90-100 ℃, the pH value of assaying reaction liquid after 20-30 minute, when treating that pH value is 6.5 left and right sides, stop to heat surplus heat and when temperature is more than 70 ℃, filter, filter out unreacted cantharidin and residue.Add the acetone solution cantharidin after leaching the thing drying, refilter, remove residue, can obtain cantharidin in the acetone soln.Its cantharidin can be used as raw material and participates in reaction once more.After above-mentioned reactant liquor leaches insoluble matter, concentrate to remove and anhydrate, can get POTASSIUM CANTHARIDATE.
The preparation of example 2 COBALT CANTHARIDATE
Press the reaction method that example 1 does not contact with air, get pure product cantharidin 4g, reagent pure cerium hydroxide cobalt 2 restrains in reactor, adds the 1000ml deionized water again.Stir, be heated to 100 ℃ of reactions after 30 minutes, stop heating, surplus heat is filtered at temperature conditions more than 70 ℃, removes unreacted reactant.Filtrate concentrates to remove and anhydrates, get final product COBALT CANTHARIDATE.
Example 3 cantharidate intravenous fluid and preparations thereof
POTASSIUM CANTHARIDATE, the cobalt salt that treating excess syndrome example 1 or example 2 are prepared or press LITHIUM CANTHARIDATE, magnesium, calcium, zinc, copper, the germanium salt of the method preparation of example 1 or 2, be dissolved in an amount of water for injection, can be mixed with the intravenous injection that contains cantharidate weight 0.00001～0.2%.Concrete grammar as: get MAGNESIUM CANTHARIDATE 0.5g and be dissolved in 1000 milliliters of waters for injection, be mixed with the intravenous injection that contains MAGNESIUM CANTHARIDATE 0.05% (for the dilution posterior vein instil with).System intravenous injection preparation process pharmacy agent routinely requires to carry out.
Example 4 cantharidate tablet and preparations thereof
Get a certain amount of cantharidate by example 3, add an amount of fully mix homogeneously such as supplementary product starch, carry out the tablet that the pelletizing press sheet coating can obtain containing cantharidate 0.05～0.6mg/ sheet again.Tablet manufacture tablet producing technology is routinely carried out.For example: get Cantharidic acid. germanium 0.1g, it is an amount of to add starch, makes 1000, enteric coatedly gets the Cantharidic acid. germanium enteric coated tablet that content is the 0.1mg/ sheet.
Example 5, the cantharidate vaginal suppository
Get a certain amount of cantharidate by example 3, adding adjuvant glycerol, gelatin and distilled water are an amount of, make suppository technology more routinely and are prepared, and can obtain containing the vaginal suppository of cantharidate 0.0005～0.06mg/g.For example: get Cantharidic acid. zinc 0.01g, glycerol adding 1500g, gelatin 1000 grams and distilled water are an amount of, at first gelatin is added the distilled water that boils in right amount and make it softening, Cantharidic acid. zinc is dissolved in the distilled water, add glycerol then, heating makes fully dissolves each other, dissolve in gelatin again, stir, 1000 of vaginal suppositories are made in the cooling molding.
Example 6 cantharidate collyrium and preparations thereof
Get a certain amount of cantharidate by example 3, the adding distilled water is an amount of, contains the collyrium of cantharidate 0.0001～0.02mg/ml by the conventional preparation method preparation of collyrium.For example: get Cantharidic acid. zinc 0.003g and be dissolved in the 1000ml distilled water, add adjuvant and can make the Cantharidic acid. zinc collyrium that contains Cantharidic acid. zinc 0.003mg/ml.
Example 7 cantharidate aerosol and preparations thereof
Get a certain amount of cantharidate by example 3, add aliphatic alcohol (for example glycerol, propylene glycol), propellant or other adjuvant are made the aerosol method routinely and can be prepared the aerosol that contains cantharidate 0.0001～0.01mg/ml.For example, get COBALT CANTHARIDATE 0.006g, be dissolved in the mixed solution of 100 milliliters of aquae destillatas, 200 milliliters of ethanol, 700 milliliters of glycerol, add an amount of propellant again and make 3000 milliliters of aerosols.This aerosol contains the 0.002mg COBALT CANTHARIDATE for every milliliter.
Cantharidate medicament by above-mentioned examples preparation can be used as the active drug of preventing and treating viral disease.Facing case history in a large number shows, use the cantharidate intravenous fluid, the cantharidate tablet is to viral hepatitis, viral enteritis, the specific therapeutical effect of viral infection such as tracheitis and condyloma acuminatum, the cantharidate vaginal suppository has good result to the infection of giving diseases prevention toxicity sexually transmitted disease condyloma, the cantharidate collyrium can be used as the specific drug of treatment and prevention pink eye disease, and the cantharidate aerosol is used to prevent and treat flu and the tracheitis that virus causes, receive effect well, in addition, the antivirus test that utilizes cell culture technology to carry out shows that the preparation that contains cantharidate has direct deactivation to HIV (human immunodeficiency virus).
The medicament of the various anti-viral uses that can be made into except that embodiment 3-7 cantharidate, cantharidate also can be made into: enteric coating glue is assisted, various types of tablet, injection and preparations such as spray and various virus disinfection that all kinds of glue are assisted agent, sugar pill, electuary, oral liquid, supp anal, smears, liniment, rubber plaster, emulsifiable paste, emulsion-type eye ointment and are used for the topical antiviral drug effect.
Claims (4)
1, a kind of cantharidate anti-virus formulation, it is characterized in that described cantharidate is lithium, potassium, magnesium, calcium, copper, zinc, cobalt or the germanium salt of Cantharidic acid., and to utilize the content (weight) that contains cantharidate in the preparation of above-mentioned cantharidate for effective ingredient be 0.00001～1%.
2, a kind of preparation method that is used for by the described preparation of claim 1 is characterized in that it being that cantharidate is made in the hydroxide of cantharidin and containing metal lithium, potassium, magnesium, calcium, copper, zinc, cobalt or germanium or oxide reaction.
3, according to the described preparation method of claim 2, it is characterized in that when water is cooked the solvent of cantharidate preparation process, when being reactant with the hydroxide of the lithium metal, the potassium that are dissolved in or are slightly soluble in water, calcium or oxide and zinc hydroxide, the consumption of cantharidin should surpass the chemical reaction equivalent, makes reactant hydrogen oxide or oxide complete reaction.
4, according to the described preparation method of claim 2, it is characterized in that when water is cooked the solvent of cantharidate preparation process, when being reactant with the hydroxide of water-fast magnesium metal, copper, cobalt or germanium or oxide and zinc oxide, the consumption of cantharidin should make reactant cantharidin energy complete reaction less than the chemical reaction equivalent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 92106087 CN1076111A (en) | 1992-03-11 | 1992-03-11 | Cantharidate anti-virus formulation and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 92106087 CN1076111A (en) | 1992-03-11 | 1992-03-11 | Cantharidate anti-virus formulation and preparation thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003043623A1 (en) * | 2001-11-23 | 2003-05-30 | Wei Wang | Antiviral, antibacterial pharmaceutical composition of cantharidic anhydride and method of preparation thereof |
| CN102093383A (en) * | 2011-01-30 | 2011-06-15 | 遵义医学院 | Potassium cantharidate and preparation method thereof |
| CN102250110A (en) * | 2011-06-03 | 2011-11-23 | 遵义医学院 | Magnesium cantharidate and preparation method thereof |
| CN102295648A (en) * | 2011-06-03 | 2011-12-28 | 遵义医学院 | Calcium cantharidinate and preparation method thereof |
| CN103479642A (en) * | 2013-09-30 | 2014-01-01 | 贵州金桥药业有限公司 | Nano sodium cantharidinate composition and preparation method thereof |
| CN103588778A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Strontium cantharidate and preparation method thereof |
| CN103588779A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Manganese cantharidate and preparation method thereof |
| CN103588780A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Barium cantharidate and preparation method thereof |
| CN103910745A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Demethylated magnesium cantharidate |
| CN103910743A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Preparation method of demethylated iron cantharidate II |
| CN103910744A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Preparation of demethylated manganese cantharidate |
| CN103923095A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Demethylated calcium cantharidate |
| CN103923098A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Preparation of demethylated strontium cantharidate |
| CN103923096A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Preparation of demethylated barium cantharidate |
-
1992
- 1992-03-11 CN CN 92106087 patent/CN1076111A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003043623A1 (en) * | 2001-11-23 | 2003-05-30 | Wei Wang | Antiviral, antibacterial pharmaceutical composition of cantharidic anhydride and method of preparation thereof |
| US8003691B2 (en) | 2001-11-23 | 2011-08-23 | Wei Wang | Antiviral and comma antibacterial pharmaceutical compositions of cantharidic anhydride and method of preparation thereof |
| CN102093383A (en) * | 2011-01-30 | 2011-06-15 | 遵义医学院 | Potassium cantharidate and preparation method thereof |
| CN102250110A (en) * | 2011-06-03 | 2011-11-23 | 遵义医学院 | Magnesium cantharidate and preparation method thereof |
| CN102295648A (en) * | 2011-06-03 | 2011-12-28 | 遵义医学院 | Calcium cantharidinate and preparation method thereof |
| CN102250110B (en) * | 2011-06-03 | 2013-04-17 | 遵义医学院 | Magnesium cantharidate and preparation method thereof |
| CN102295648B (en) * | 2011-06-03 | 2013-04-17 | 遵义医学院 | Calcium cantharidinate and preparation method thereof |
| CN103479642A (en) * | 2013-09-30 | 2014-01-01 | 贵州金桥药业有限公司 | Nano sodium cantharidinate composition and preparation method thereof |
| CN103588778A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Strontium cantharidate and preparation method thereof |
| CN103588779A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Manganese cantharidate and preparation method thereof |
| CN103588780A (en) * | 2013-11-15 | 2014-02-19 | 遵义医学院 | Barium cantharidate and preparation method thereof |
| CN103910745A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Demethylated magnesium cantharidate |
| CN103910743A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Preparation method of demethylated iron cantharidate II |
| CN103910744A (en) * | 2014-04-23 | 2014-07-09 | 遵义医学院 | Preparation of demethylated manganese cantharidate |
| CN103923095A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Demethylated calcium cantharidate |
| CN103923098A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Preparation of demethylated strontium cantharidate |
| CN103923096A (en) * | 2014-04-23 | 2014-07-16 | 遵义医学院 | Preparation of demethylated barium cantharidate |
| CN103910745B (en) * | 2014-04-23 | 2017-01-18 | 遵义医学院 | Demethylated magnesium cantharidate |
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