CN104163773B - 一种四环素的精制方法 - Google Patents
一种四环素的精制方法 Download PDFInfo
- Publication number
- CN104163773B CN104163773B CN201310391365.7A CN201310391365A CN104163773B CN 104163773 B CN104163773 B CN 104163773B CN 201310391365 A CN201310391365 A CN 201310391365A CN 104163773 B CN104163773 B CN 104163773B
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- CN
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- Prior art keywords
- tsiklomitsin
- purification
- mixture
- liquor
- filter cake
- Prior art date
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- NWXMGUDVXFXRIG-WESIUVDSSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide Chemical compound C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O NWXMGUDVXFXRIG-WESIUVDSSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000000746 purification Methods 0.000 title claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 239000012065 filter cake Substances 0.000 claims abstract description 24
- 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 abstract description 17
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 17
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 17
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 13
- 229910021538 borax Inorganic materials 0.000 claims abstract description 12
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 12
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000003916 acid precipitation Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000007670 refining Methods 0.000 claims description 11
- 238000005352 clarification Methods 0.000 claims description 10
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical group [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 239000000243 solution Substances 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
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 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
- 239000004098 Tetracycline Substances 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 150000001408 amides Chemical class 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
- 238000010812 external standard method Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 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
- 239000013049 sediment Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
项目 | 实施例1 | 实施例2 | 实施例3 |
收率(%) | 93.4 | 94.5 | 93.8 |
纯度(%) | 99.2 | 99.4 | 99.7 |
Claims (8)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201310391365.7A CN104163773B (zh) | 2013-08-30 | 2013-08-30 | 一种四环素的精制方法 |
Applications Claiming Priority (1)
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CN201310391365.7A CN104163773B (zh) | 2013-08-30 | 2013-08-30 | 一种四环素的精制方法 |
Publications (2)
Publication Number | Publication Date |
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CN104163773A CN104163773A (zh) | 2014-11-26 |
CN104163773B true CN104163773B (zh) | 2016-04-27 |
Family
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Family Applications (1)
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CN201310391365.7A Active CN104163773B (zh) | 2013-08-30 | 2013-08-30 | 一种四环素的精制方法 |
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CN (1) | CN104163773B (zh) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106543019A (zh) * | 2016-11-10 | 2017-03-29 | 聊城大学 | 一种无水四环素无定型物的制备方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4659515A (en) * | 1983-09-02 | 1987-04-21 | Chinoin Gyogyszer Es Vegyeszeti Termekek Gyara Rt | Process for the preparation of 6-demethyl-6-deoxy-6-methylene-5-oxytetracyclin and the 11A-chloro-derivative thereof |
CN1244523A (zh) * | 1998-08-10 | 2000-02-16 | 清华大学 | 用醇类溶剂提取和纯化四环类抗生素 |
CN1932023A (zh) * | 2005-09-14 | 2007-03-21 | 凯能高科技工程(上海)有限公司 | 四环类抗生素清洁生产工艺 |
CN102796024A (zh) * | 2012-08-29 | 2012-11-28 | 郑州后羿制药有限公司 | 一种土霉素的精制方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2013046572A (ja) * | 2009-12-08 | 2013-03-07 | Kaneka Corp | 光学活性2−ヒドロキシシクロアルカンカルボン酸エステルの製造方法 |
-
2013
- 2013-08-30 CN CN201310391365.7A patent/CN104163773B/zh active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4659515A (en) * | 1983-09-02 | 1987-04-21 | Chinoin Gyogyszer Es Vegyeszeti Termekek Gyara Rt | Process for the preparation of 6-demethyl-6-deoxy-6-methylene-5-oxytetracyclin and the 11A-chloro-derivative thereof |
CN1244523A (zh) * | 1998-08-10 | 2000-02-16 | 清华大学 | 用醇类溶剂提取和纯化四环类抗生素 |
CN1932023A (zh) * | 2005-09-14 | 2007-03-21 | 凯能高科技工程(上海)有限公司 | 四环类抗生素清洁生产工艺 |
CN102796024A (zh) * | 2012-08-29 | 2012-11-28 | 郑州后羿制药有限公司 | 一种土霉素的精制方法 |
Non-Patent Citations (1)
Title |
---|
四环素精制工段的设计;邱毓存;《工厂设计》;19841231;第9页右栏第2段 * |
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CN104163773A (zh) | 2014-11-26 |
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Inventor after: Zhang Tingpan Inventor after: Li Yae Inventor after: Li Jianzheng Inventor after: Wang Pei Inventor before: Zhang Tingpan Inventor before: Li Yae Inventor before: Li Jianzheng |
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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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Denomination of invention: Refining method for tetracycline Effective date of registration: 20200629 Granted publication date: 20160427 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 tetracycline Effective date of registration: 20220622 Granted publication date: 20160427 Pledgee: Zhumadian Rural Commercial Bank Co.,Ltd. Pledgor: HENAN HOUYI PHARMACY CO.,LTD. Registration number: Y2022980008586 |
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