CN102161693A - Preparation method of zinc bacitracin - Google Patents
Preparation method of zinc bacitracin Download PDFInfo
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- CN102161693A CN102161693A CN201010606575XA CN201010606575A CN102161693A CN 102161693 A CN102161693 A CN 102161693A CN 201010606575X A CN201010606575X A CN 201010606575XA CN 201010606575 A CN201010606575 A CN 201010606575A CN 102161693 A CN102161693 A CN 102161693A
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Abstract
The invention discloses a preparation method of zinc bacitracin, which is characterized by comprising the following steps: adding an alkaline solution into a bacitracin solution; adjusting pH to 8-11; adding inorganic zinc to form a salt; adjusting pH to 5-7; stirring for 1-2 hours; standing for 5-10 hours; and separating, drying, smashing, screening, checking, and packaging finished products to obtain qualified zinc bacitracin. The preparation method has the characteristics of high efficiency, simple equipment, good economy, high purity, low energy consumption and the like, can be continuously operated at normal temperature and is especially suitable for industrial mass production of the zinc bacitracin.
Description
Technical field:
The invention belongs to organic chemistry filed, relate to a kind of in solution the general preparation method of peptide, specifically, relate to a kind of method that in bacitracin solution, prepares Zinc-bacitracin.It is a raw material with the bacitracin fermented liquid, it is taked chemistry and physical methods such as separation, extraction, finally obtains Zinc-bacitracin.
Background technology:
(Bacitracin zinc is abbreviated as BcZn to Zinc-bacitracin, CAS1405-89-6) is the complex compound of a kind of zinc and bacitracin, is white or off-white powder, and special smelly, bitter is arranged.This material is almost insoluble in water, methyl alcohol, acetone, chloroform, and is soluble in the pyridine slightly soluble in ether.Zinc-bacitracin is a kind of effective narrow spectrum peptide antibiotics, its antimicrobial spectrum and penicillins are seemingly, be primarily aimed at gram-positive cocci and bacillus, minority Gram-negative bacteria, spirochete and actinomycetes are also had certain restraining effect, have advantages such as efficient, low toxicity, less residue.Therefore, Zinc-bacitracin is not only a kind of important antibiotic medicine, also is the good livestock and poultry antibiotic feed additive of security.
Zinc-bacitracin is Zn
2+The complex compound that forms with the carboxylicesters of the sulphur atom of the δ-N of the imidazolyl of the Histidine of bacitracin, thiazoline ring and L-glutamic acid.
Existing Zinc-bacitracin production technology mainly prepares by microbe fermentation method, with subtilis (Bacillus subtilis) and category-B Bacillus licheniformis (Bacillus licheniformis) fermented liquid is raw material, fermented liquid is with after zinc oxide or zinc chloride mix, vacuum-evaporation concentrates, make the butt substances content bring up to 17%～20%, the spray-dried again Zinc-bacitracin that obtains from 4.5%～5%.The product component complexity that this method obtains can only be used for fodder additives.
U.S. Pat 2809892 discloses the method that a kind of water miscible zinc salt prepares Zinc-bacitracin, zinc salt is joined in the bacitracin fermented liquid after the acidifying, improve the pH value of mixture, Zinc-bacitracin is precipitated out, isolate the Zinc-bacitracin complex compound, carry out drying again, there is the problem of the co-precipitation of metal hydroxides in this method, and bacitracin content is no more than 4%～8%.U.S. Pat 393769 discloses a kind of method that zinc hydroxide prepares Zinc-bacitracin that do not contain, but lower with the excessive zine ion yield of ammonia radical ion complexing.
The preparation method of Zinc-bacitracin is many, and still, these methods are used in the industrial production, all has many difficulties.
Summary of the invention:
Characteristics such as the preparation method who the purpose of this invention is to provide a kind of Zinc-bacitracin, this method have that efficient height, equipment are simple, good economy performance, purity height, energy consumption are low, operate continuously at normal temperatures are particularly suitable for suitability for industrialized production.
The present invention realizes as follows:
In bacitracin solution, add basic solution, regulate PH=8～11, add the inorganic zinc salify, regulate PH=5～7, stirred 1～2 hour, left standstill 5～10 hours with mineral acid.Obtain qualified Zinc-bacitracin by production stages such as separation, drying, pulverizing, screening, check, finished product packings then.Described bacitracin solution is to tire greater than 5000u/ml, and electricity is led the extraction separation solution less than the subtilis of 2000 μ s/cm (Bacillus subtilis) and category-B Bacillus licheniformis (Bacillus licheniformis) fermented liquid.
Described basic solution is a kind of in ammoniacal liquor, the sodium hydroxide.
Described inorganic zinc is a kind of of zinc oxide, zinc chloride, zinc sulfate.
Described mineral acid is that hydrochloric acid, vitriolic are a kind of.
The zinc content of the Zinc-bacitracin that the inventive method makes is 4.0～6.0%, and Bacitracin A content is greater than 40.0%, Bacitracin A, B
1, B
2And B
3Total amount greater than 70.0%, tire greater than 65U/g.
The Zinc-bacitracin that the inventive method makes is directly as the raw material of preparations such as medical injection agent, ointment.
Embodiment:
Embodiment one
In 100L bacitracin solution, add the 1.5M sodium hydroxide solution, regulate PH=8～11, add 2.3Kg 30% liquor zinci chloridi salify, regulate PH=5～7, stirred 1～2 hour, left standstill 6～7 hours with hydrochloric acid.The fluidized drying case of packing into after separating by whizzer again carries out drying, obtains Zinc-bacitracin 11.2Kg.
Embodiment two
In 100L bacitracin solution, add the 1.5M sodium hydroxide solution, regulate PH=8～11, add 3.2Kg 30% solution of zinc sulfate salify, regulate PH=5～7, stirred 1～2 hour, left standstill 6～7 hours with hydrochloric acid.The fluidized drying case of packing into after separating by whizzer again carries out drying, obtains Zinc-bacitracin 12.6Kg.
Embodiment three
In 100L bacitracin solution, add the 1.5M sodium hydroxide solution, regulate PH=8～11, add 3.2Kg 30% solution of zinc sulfate salify, regulate PH=5～7, stirred 1～2 hour, left standstill 6～7 hours with sulfuric acid.The fluidized drying case of packing into after separating by whizzer again carries out drying, obtains Zinc-bacitracin 11.3Kg.
Embodiment four
In 100L bacitracin solution, add the 1.5M sodium hydroxide solution, regulate PH=8～11, add 1.9Kg zinc oxide and 7.5Kg water, stirred 2 hours, regulate PH=5～7, stirred 1～2 hour, left standstill 6～7 hours with sulfuric acid.The fluidized drying case of packing into after separating by whizzer again carries out drying, obtains Zinc-bacitracin 9.8Kg.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand, and the present invention is not limited to particular example as described herein and embodiment.The purpose that comprises these particular example and embodiment here is to help those of skill in the art to put into practice the present invention.Any those of skill in the art are easy to be further improved without departing from the spirit and scope of the present invention and perfect, therefore, the present invention only is subjected to the restriction of the content and the scope of claim of the present invention, and its intention contains interior alternatives and the equivalent of spirit and scope of the invention that all authority requirement is limited.
Claims (6)
1. the preparation method of a Zinc-bacitracin.Its characterization step is as follows:
In bacitracin solution, add basic solution, regulate PH=8～11, add the inorganic zinc salify, regulate PH=5～7, stirred 1～2 hour, left standstill 5～10 hours with mineral acid.Obtain qualified Zinc-bacitracin by production stages such as separation, drying, pulverizing, screening, check, finished product packings then.
2. the preparation method of Zinc-bacitracin according to claim 1, it is characterized in that described bacitracin solution is to tire greater than 5000u/ml, electricity is led the extraction separation solution less than the subtilis of 2000 μ s/cm (Bacillus subtilis) and category-B Bacillus licheniformis (Bacillus licheniformis) fermented liquid.
3. the preparation method of Zinc-bacitracin according to claim 1 is characterized in that described basic solution is a kind of in ammoniacal liquor, the sodium hydroxide.
4. the preparation method of Zinc-bacitracin according to claim 1 is characterized in that described inorganic zinc is a kind of in zinc oxide, zinc chloride, the zinc sulfate.
5. the preparation method of Zinc-bacitracin according to claim 1 is characterized in that described mineral acid is a kind of in hydrochloric acid, the sulfuric acid.
6. the preparation method of Zinc-bacitracin according to claim 1, the zinc content that it is characterized in that described Zinc-bacitracin is 4.0～6.0%, Bacitracin A content is greater than 40.0%, Bacitracin A, B
1, B
2And B
3Total amount greater than 70.0%, tire greater than 65U/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010606575XA CN102161693A (en) | 2010-12-27 | 2010-12-27 | Preparation method of zinc bacitracin |
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| CN201010606575XA CN102161693A (en) | 2010-12-27 | 2010-12-27 | Preparation method of zinc bacitracin |
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| CN201010606575XA Pending CN102161693A (en) | 2010-12-27 | 2010-12-27 | Preparation method of zinc bacitracin |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102488709A (en) * | 2011-12-28 | 2012-06-13 | 广州市和生堂动物药业有限公司 | Florfenicol-zinc chelate injection and preparation method thereof |
| CN104621360A (en) * | 2015-03-11 | 2015-05-20 | 河北圣雪大成制药有限责任公司 | Preparation method of bacitracin zinc premix |
| CN105566458A (en) * | 2016-02-23 | 2016-05-11 | 华北制药集团新药研究开发有限责任公司 | Method for preparing bacitracin and method for preparing zinc salt of bacitracin |
| CN105616387A (en) * | 2016-01-23 | 2016-06-01 | 雅赛利(台州)制药有限公司 | Zinc bacitracin |
| CN106359898A (en) * | 2016-08-30 | 2017-02-01 | 齐鲁制药（内蒙古）有限公司 | Preparation method of bacitracin zinc premixing agent |
| CN106729613A (en) * | 2016-12-29 | 2017-05-31 | 山东宝利甾体生物科技有限公司 | A kind of method of efficient concentration Bacitracin Zinc zymotic fluid |
| CN109608522A (en) * | 2018-11-23 | 2019-04-12 | 江苏九阳生物制药有限公司 | A kind of method of fermenting and producing bacitracin |
| CN113801204A (en) * | 2021-08-19 | 2021-12-17 | 江苏九阳生物制药有限公司 | Preparation method of bacitracin zinc |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2809892A (en) * | 1954-11-01 | 1957-10-15 | Commerical Solvents Corp | Zinc bacitracin feed supplement |
| US4164572A (en) * | 1976-10-06 | 1979-08-14 | A/S Apothekernes Laboratorium For Specialpraeparater | Zinc bacitracin composition for use as a feed supplement and method for making the same |
-
2010
- 2010-12-27 CN CN201010606575XA patent/CN102161693A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2809892A (en) * | 1954-11-01 | 1957-10-15 | Commerical Solvents Corp | Zinc bacitracin feed supplement |
| US4164572A (en) * | 1976-10-06 | 1979-08-14 | A/S Apothekernes Laboratorium For Specialpraeparater | Zinc bacitracin composition for use as a feed supplement and method for making the same |
Non-Patent Citations (1)
| Title |
|---|
| 刘咏: "抗生素杆菌肽锌脱色提纯工艺研究", 《中国优秀硕士学位论文全文数据库工程科技辑I辑》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102488709A (en) * | 2011-12-28 | 2012-06-13 | 广州市和生堂动物药业有限公司 | Florfenicol-zinc chelate injection and preparation method thereof |
| CN102488709B (en) * | 2011-12-28 | 2013-10-30 | 广州市和生堂动物药业有限公司 | Florfenicol-zinc chelate injection and preparation method thereof |
| CN104621360A (en) * | 2015-03-11 | 2015-05-20 | 河北圣雪大成制药有限责任公司 | Preparation method of bacitracin zinc premix |
| CN105616387A (en) * | 2016-01-23 | 2016-06-01 | 雅赛利(台州)制药有限公司 | Zinc bacitracin |
| CN105616387B (en) * | 2016-01-23 | 2018-10-09 | 雅赛利(台州)制药有限公司 | Bacitracin Zinc |
| CN105566458A (en) * | 2016-02-23 | 2016-05-11 | 华北制药集团新药研究开发有限责任公司 | Method for preparing bacitracin and method for preparing zinc salt of bacitracin |
| CN106359898A (en) * | 2016-08-30 | 2017-02-01 | 齐鲁制药（内蒙古）有限公司 | Preparation method of bacitracin zinc premixing agent |
| CN106729613A (en) * | 2016-12-29 | 2017-05-31 | 山东宝利甾体生物科技有限公司 | A kind of method of efficient concentration Bacitracin Zinc zymotic fluid |
| CN109608522A (en) * | 2018-11-23 | 2019-04-12 | 江苏九阳生物制药有限公司 | A kind of method of fermenting and producing bacitracin |
| CN109608522B (en) * | 2018-11-23 | 2022-11-18 | 江苏九阳生物制药有限公司 | Method for producing bacitracin by fermentation |
| CN113801204A (en) * | 2021-08-19 | 2021-12-17 | 江苏九阳生物制药有限公司 | Preparation method of bacitracin zinc |
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Application publication date: 20110824 |