CN102796024B - 一种土霉素的精制方法 - Google Patents
一种土霉素的精制方法 Download PDFInfo
- Publication number
- CN102796024B CN102796024B CN201210312189.9A CN201210312189A CN102796024B CN 102796024 B CN102796024 B CN 102796024B CN 201210312189 A CN201210312189 A CN 201210312189A CN 102796024 B CN102796024 B CN 102796024B
- Authority
- CN
- China
- Prior art keywords
- terramycin
- hydrochloric acid
- refining
- filtrate
- oxytetracycline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000007670 refining Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000004100 Oxytetracycline Substances 0.000 title abstract 6
- IWVCMVBTMGNXQD-PXOLEDIWSA-N oxytetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3[C@H](O)[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-PXOLEDIWSA-N 0.000 title abstract 6
- 229960000625 oxytetracycline Drugs 0.000 title abstract 6
- 235000019366 oxytetracycline Nutrition 0.000 title abstract 6
- IWVCMVBTMGNXQD-UHFFFAOYSA-N terramycin dehydrate Natural products C1=CC=C2C(O)(C)C3C(O)C4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O IWVCMVBTMGNXQD-UHFFFAOYSA-N 0.000 title abstract 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 8
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract 5
- KIPLYOUQVMMOHB-MXWBXKMOSA-L [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O Chemical compound [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O KIPLYOUQVMMOHB-MXWBXKMOSA-L 0.000 claims description 55
- 229940063650 terramycin Drugs 0.000 claims description 55
- 239000012065 filter cake Substances 0.000 claims description 20
- 238000000746 purification Methods 0.000 claims description 12
- 238000005352 clarification Methods 0.000 claims description 8
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 239000002516 radical scavenger Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 239000013558 reference substance Substances 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000010812 external standard method Methods 0.000 description 3
- 238000004811 liquid chromatography Methods 0.000 description 3
- 238000013094 purity test Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- -1 leave standstill 4h Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- UHHHTIKWXBRCLT-VDBOFHIQSA-N (4s,4ar,5s,5ar,6r,12ar)-4-(dimethylamino)-1,5,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4a,5,5a,6-tetrahydro-4h-tetracene-2-carboxamide;ethanol;hydrate;dihydrochloride Chemical compound O.Cl.Cl.CCO.C1=CC=C2[C@H](C)[C@@H]([C@H](O)[C@@H]3[C@](C(O)=C(C(N)=O)C(=O)[C@H]3N(C)C)(O)C3=O)C3=C(O)C2=C1O.C1=CC=C2[C@H](C)[C@@H]([C@H](O)[C@@H]3[C@](C(O)=C(C(N)=O)C(=O)[C@H]3N(C)C)(O)C3=O)C3=C(O)C2=C1O UHHHTIKWXBRCLT-VDBOFHIQSA-N 0.000 description 1
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 241000204031 Mycoplasma Species 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 241000606701 Rickettsia Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QZIQJVCYUQZDIR-UHFFFAOYSA-N mechlorethamine hydrochloride Chemical compound Cl.ClCCN(C)CCCl QZIQJVCYUQZDIR-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 229940063678 vibramycin Drugs 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
实施例1 | 实施例2 | 实施例3 | |
含量(%) | 99.4 | 99.6 | 99.9 |
Claims (4)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201210312189.9A CN102796024B (zh) | 2012-08-29 | 2012-08-29 | 一种土霉素的精制方法 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201210312189.9A CN102796024B (zh) | 2012-08-29 | 2012-08-29 | 一种土霉素的精制方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102796024A CN102796024A (zh) | 2012-11-28 |
CN102796024B true CN102796024B (zh) | 2014-07-30 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201210312189.9A Active CN102796024B (zh) | 2012-08-29 | 2012-08-29 | 一种土霉素的精制方法 |
Country Status (1)
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CN (1) | CN102796024B (zh) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104163773B (zh) * | 2013-08-30 | 2016-04-27 | 郑州后羿制药有限公司 | 一种四环素的精制方法 |
CN107011204B (zh) * | 2017-04-12 | 2019-10-01 | 扬州联博药业有限公司 | 一种从盐酸土霉素结晶母液中回收盐酸土霉素的方法 |
CN116621724B (zh) * | 2023-07-21 | 2023-10-27 | 山东国邦药业有限公司 | 一种降低杂质2-乙酰-2-去酰胺土霉素含量的土霉素提取方法 |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101921211A (zh) * | 2010-08-17 | 2010-12-22 | 郑州后羿制药有限公司 | 一种土霉素碱的提纯方法 |
-
2012
- 2012-08-29 CN CN201210312189.9A patent/CN102796024B/zh active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101921211A (zh) * | 2010-08-17 | 2010-12-22 | 郑州后羿制药有限公司 | 一种土霉素碱的提纯方法 |
Non-Patent Citations (2)
Title |
---|
李十中等.高纯度土霉素碱生产工艺研究(I).《中国抗生素杂志》.2000,第25卷(第5期), |
高纯度土霉素碱生产工艺研究(I);李十中等;《中国抗生素杂志》;20001031;第25卷(第5期);第344-345页,394页 * |
Also Published As
Publication number | Publication date |
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CN102796024A (zh) | 2012-11-28 |
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Address after: 451161 Zhengzhou economic comprehensive experimentation area, Zhengzhou air port, Henan, Xingang Province Patentee after: HENAN HOUYI INDUSTRIAL GROUP CO.,LTD. Address before: 451162 Xingang, Henan, Zhengzhou, Hong Kong airport on the eastern side of the road on the eastern side of Zhengzhou Patentee before: ZHENGZHOU HOUYI PHARMACEUTICAL Co.,Ltd. |
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Effective date of registration: 20160927 Address after: 463000 Industrial Park, industrial agglomeration area, Henan, Zhumadian (No. two industrial road, No. 1) Patentee after: HENAN HOUYI PHARMACY CO.,LTD. Address before: 451161 Zhengzhou economic comprehensive experimentation area, Zhengzhou air port, Henan, Xingang Province Patentee before: HENAN HOUYI INDUSTRIAL GROUP CO.,LTD. |
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Denomination of invention: Method for refining oxytetracycline Effective date of registration: 20190618 Granted publication date: 20140730 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY CO.,LTD. Registration number: 2019410000016 |
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Date of cancellation: 20200628 Granted publication date: 20140730 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY Co.,Ltd. Registration number: 2019410000016 |
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PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Method for refining oxytetracycline Effective date of registration: 20200629 Granted publication date: 20140730 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY Co.,Ltd. Registration number: Y2020980003549 |
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Date of cancellation: 20220621 Granted publication date: 20140730 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY CO.,LTD. Registration number: Y2020980003549 |
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Denomination of invention: A refining method of Oxytetracycline Effective date of registration: 20220622 Granted publication date: 20140730 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY CO.,LTD. Registration number: Y2022980008586 |