CN1374310A - Prepn process of sodium cantharidinate - Google Patents
Prepn process of sodium cantharidinate Download PDFInfo
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- CN1374310A CN1374310A CN 02113490 CN02113490A CN1374310A CN 1374310 A CN1374310 A CN 1374310A CN 02113490 CN02113490 CN 02113490 CN 02113490 A CN02113490 A CN 02113490A CN 1374310 A CN1374310 A CN 1374310A
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- cantharidin
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Abstract
The present invention discloses the preparation process of disodium cantharidinate. The preparation process includes the steps of cantharidin extraction recrystallization and preparation of disodium cantharidinate. Disodium cantharidinate may be used in preparing antineoplastic medicine in various forms, including injection, infusion, tablet, capsule, oral liquor, etc.
Description
The present invention is a kind of preparation technology of disodium cantharidinate.
Disodium cantharidinate is as antineoplastic pioneer's medicine, make the application modern biotechnology from cantharis, extract its effective constituent, the bound drug synthetic technology, through synthesizing, make with extra care, being transformed, its anticancer mechanism mainly is the protein synthesis of anticancer, influence its RNA and DNA, the growth division of final anticancer.The preparation technology of disodium cantharidinate raw material does not see so far the document record.
The objective of the invention is: provide a kind of with the Chinese blister beetle polypide through extract Cantharidin, recrystallization, produce and the technology of disodium cantharidinate elaboration.
The present invention is achieved in that it comprises that Cantharidin extracts, recrystallization, and several steps of preparation disodium cantharidinate:
(1) gets Chinese blister beetle polypide powder earlier and place container, add hydrochloric acid and soaked into 24 hours, add the acetone cold soaking again, shake up, soaked 72 hours, filter, filtrate places separating funnel, divide and get organic phase, put water-bath and reclaim acetone, add the washing of sherwood oil and dehydrated alcohol mixing solutions while hot to the ointment shape, through suction filtration, discard washings, with sherwood oil and dehydrated alcohol mixed solution cleaning product several, get yellow-white Cantharidin crude product again;
(2) get the ratio adding acetone soln of Cantharidin crude product in 1: 30 weight, make its dissolving in the heating in water bath backflow, treat that it dissolves the gac of back adding 0.3% fully, refluxed 30 minutes, suction filtration gets achromatism and clarity filtrate while hot, filtrate is placed flask, reclaim acetone to 1/5 of original volume, cooling back suction filtration gets white crystals;
(3) get the ratio adding acetone soln of Cantharidin elaboration in 1: 20 weight, heating in water bath refluxes and makes its dissolving, get simultaneously with the Cantharidin mol ratio be that to make concentration be 20% solution for 1: 2 sodium hydroxide adding distil water, treat that Cantharidin dissolves the back fully and adds sodium hydroxide solution reaction 1 hour, use water distilling apparatus instead and steam acetone to doing, the gac of adding 0.3%, refluxed 10 minutes, suction filtration while hot, get water white transparency filtrate, filtrate is diluted to original 10 times, put water-bath and concentrate, drying gets white crystalline powder.
The present invention has that technology is reasonable, simple and practical, security is good, the finished product stable in properties of preparation, and the purity height is easy to advantages such as detection by quality standard.Can be applicable to the antitumor drug production of multiple formulations such as injection, infusion solutions, tablet, capsule, granule, oral liquid and ointment.
Embodiments of the invention:
(1) gets Chinese blister beetle polypide powder 1kg, place the tool plug container of 10000ml, add hydrochloric acid and soaked into 24 hours, add acetone (or chloroform) cold soaking again, shake up, soaked 72 hours, filter, filtrate places separating funnel, divides and gets organic phase, put water-bath and reclaim acetone to the ointment shape, add sherwood oil and dehydrated alcohol (1: 1) mixing solutions while hot and wash in right amount,, discard washings through suction filtration, with sherwood oil and an amount of cleaning product several of dehydrated alcohol (1: 1) mixed solution, get yellow-white Cantharidin crude product again;
(2) get the ratio adding acetone soln of Cantharidin crude product in 1: 30 weight, make its dissolving in the heating in water bath backflow, treat that it dissolves the gac of back adding 0.3% fully, refluxed 30 minutes, suction filtration gets achromatism and clarity filtrate while hot, filtrate is placed round-bottomed flask, reclaim acetone to 1/5 of original volume, be positioned over suction filtration next day (filtrate preservation), get white crystals;
(3) get the ratio adding acetone soln of Cantharidin elaboration in 1: 20 weight, heating in water bath refluxes and makes its dissolving, get simultaneously with the Cantharidin mol ratio be that to make concentration be 20% solution for 1: 2 sodium hydroxide adding distil water, after treating that Cantharidin dissolves fully, add the sodium hydroxide solution that configures, reacted 1 hour, use water distilling apparatus instead and steam acetone, add 0.3% gac, refluxed 10 minutes to doing, suction filtration while hot, get water white transparency filtrate, filtrate is diluted to original 10 times, put water-bath and concentrate, drying gets white crystalline powder and is the disodium cantharidinate elaboration.
Claims (1)
1, a kind of preparation technology of disodium cantharidinate, it comprises that Cantharidin extracts, recrystallization, several steps of preparation disodium cantharidinate is characterized in that:
(1) gets Chinese blister beetle polypide powder earlier and place container, add hydrochloric acid and soaked into 24 hours, add the acetone cold soaking again, shake up, soaked 72 hours, filter, filtrate places separating funnel, divide and get organic phase, put water-bath and reclaim acetone, add the washing of sherwood oil and dehydrated alcohol mixing solutions while hot to the ointment shape, through suction filtration, discard washings, with sherwood oil and dehydrated alcohol mixed solution cleaning product several, get yellow-white Cantharidin crude product again;
(2) get the ratio adding acetone soln of Cantharidin crude product in 1: 30 weight, make its dissolving in the heating in water bath backflow, treat that it dissolves the gac of back adding 0.3% fully, refluxed 30 minutes, suction filtration gets achromatism and clarity filtrate while hot, filtrate is placed flask, reclaim acetone to 1/5 of original volume, cooling back suction filtration gets white crystals;
(3) get the ratio adding acetone soln of Cantharidin elaboration in 1: 20 weight, heating in water bath refluxes and makes its dissolving, get simultaneously with the Cantharidin mol ratio be that to make concentration be 20% solution for 1: 2 sodium hydroxide adding distil water, treat that Cantharidin dissolves the back fully and adds sodium hydroxide solution reaction 1 hour, use water distilling apparatus instead and steam acetone to doing, the gac of adding 0.3%, refluxed 10 minutes, suction filtration while hot, get water white transparency filtrate, filtrate is diluted to original 10 times, put water-bath and concentrate, drying gets white crystalline powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021134901A CN1166669C (en) | 2002-03-20 | 2002-03-20 | Prepn process of sodium cantharidinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021134901A CN1166669C (en) | 2002-03-20 | 2002-03-20 | Prepn process of sodium cantharidinate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1374310A true CN1374310A (en) | 2002-10-16 |
| CN1166669C CN1166669C (en) | 2004-09-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021134901A Expired - Lifetime CN1166669C (en) | 2002-03-20 | 2002-03-20 | Prepn process of sodium cantharidinate |
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| CN (1) | CN1166669C (en) |
Cited By (10)
| 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 |
| CN101108853B (en) * | 2007-07-27 | 2010-05-26 | 贵州大学 | Separation purification process of cantharidin |
| CN101108854B (en) * | 2007-07-27 | 2010-05-26 | 贵州大学 | Separation purification process of cantharidin |
| CN102146086A (en) * | 2011-04-12 | 2011-08-10 | 贵州金桥药业有限公司 | Preparation method of sodium cantharidate |
| CN102268006A (en) * | 2011-06-15 | 2011-12-07 | 北京联合大学生物化学工程学院 | Method for extracting cantharidin from compound enzyme |
| CN102276619A (en) * | 2011-06-21 | 2011-12-14 | 贵州金桥药业有限公司 | Method for preparing sodium canthanridate |
| CN102336765A (en) * | 2011-10-11 | 2012-02-01 | 江苏四环生物股份有限公司 | Method for extracting cantharidin from cantharides |
| CN102796794A (en) * | 2012-08-31 | 2012-11-28 | 哈尔滨工业大学 | Preparation method of cantharis toxin |
| 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 |
| CN108250210A (en) * | 2017-11-29 | 2018-07-06 | 江蓓 | A kind of disodium cantharidinate and preparation method thereof |
-
2002
- 2002-03-20 CN CNB021134901A patent/CN1166669C/en not_active Expired - Lifetime
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8003691B2 (en) | 2001-11-23 | 2011-08-23 | Wei Wang | Antiviral and comma antibacterial pharmaceutical compositions of cantharidic anhydride and method of preparation thereof |
| WO2003043623A1 (en) * | 2001-11-23 | 2003-05-30 | Wei Wang | Antiviral, antibacterial pharmaceutical composition of cantharidic anhydride and method of preparation thereof |
| CN101108853B (en) * | 2007-07-27 | 2010-05-26 | 贵州大学 | Separation purification process of cantharidin |
| CN101108854B (en) * | 2007-07-27 | 2010-05-26 | 贵州大学 | Separation purification process of cantharidin |
| CN102146086B (en) * | 2011-04-12 | 2012-03-07 | 贵州金桥药业有限公司 | Preparation method of sodium cantharidate |
| CN102146086A (en) * | 2011-04-12 | 2011-08-10 | 贵州金桥药业有限公司 | Preparation method of sodium cantharidate |
| CN102268006A (en) * | 2011-06-15 | 2011-12-07 | 北京联合大学生物化学工程学院 | Method for extracting cantharidin from compound enzyme |
| CN102268006B (en) * | 2011-06-15 | 2013-08-14 | 北京联合大学生物化学工程学院 | Method for extracting cantharidin from compound enzyme |
| CN102276619A (en) * | 2011-06-21 | 2011-12-14 | 贵州金桥药业有限公司 | Method for preparing sodium canthanridate |
| CN102336765A (en) * | 2011-10-11 | 2012-02-01 | 江苏四环生物股份有限公司 | Method for extracting cantharidin from cantharides |
| CN102796794A (en) * | 2012-08-31 | 2012-11-28 | 哈尔滨工业大学 | Preparation method of cantharis toxin |
| 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 |
| CN108250210A (en) * | 2017-11-29 | 2018-07-06 | 江蓓 | A kind of disodium cantharidinate and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1166669C (en) | 2004-09-15 |
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Assignee: Guizhou Baiqiang Pharmaceutical Co., Ltd. Assignor: Guizhou Junzhitang Pharmaceutical Co., Ltd. Contract record no.: 2011520000004 Denomination of invention: Preparing process of sodium cantharidinate Granted publication date: 20040915 License type: Exclusive License Open date: 20021016 Record date: 20110725 |
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| TR01 | Transfer of patent right |
Effective date of registration: 20170616 Address after: 550002 N-10, industrial zone, Nanming District, Guizhou, Guiyang Patentee after: Guizhou Baiqiang Pharmaceutical Co., Ltd. Address before: 550001 No. 85 Zhonghua Road, Guiyang, Guizhou Patentee before: Guizhou Junzhitang Pharmaceutical Co., Ltd. |
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