CN1840537A - 高纯度灯盏花乙素原料药的制备工艺 - Google Patents
高纯度灯盏花乙素原料药的制备工艺 Download PDFInfo
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- CN1840537A CN1840537A CN 200510010723 CN200510010723A CN1840537A CN 1840537 A CN1840537 A CN 1840537A CN 200510010723 CN200510010723 CN 200510010723 CN 200510010723 A CN200510010723 A CN 200510010723A CN 1840537 A CN1840537 A CN 1840537A
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- lamp
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- raw material
- dish flower
- flower acetic
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- 239000002994 raw material Substances 0.000 title claims description 13
- DJSISFGPUUYILV-UHFFFAOYSA-N UNPD161792 Natural products O1C(C(O)=O)C(O)C(O)C(O)C1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 DJSISFGPUUYILV-UHFFFAOYSA-N 0.000 title abstract description 9
- DJSISFGPUUYILV-ZFORQUDYSA-N scutellarin Chemical compound O1[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1OC(C(=C1O)O)=CC2=C1C(=O)C=C(C=1C=CC(O)=CC=1)O2 DJSISFGPUUYILV-ZFORQUDYSA-N 0.000 title abstract description 9
- NPLTVGMLNDMOQE-UHFFFAOYSA-N carthamidin Natural products C1=CC(O)=CC=C1C1OC2=CC(O)=C(O)C(O)=C2C(=O)C1 NPLTVGMLNDMOQE-UHFFFAOYSA-N 0.000 title abstract description 8
- 229930190376 scutellarin Natural products 0.000 title abstract description 8
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000003814 drug Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 17
- 238000005516 engineering process Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000001556 precipitation Methods 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- -1 amido methane Chemical compound 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- TYJOJLOWRIQYQM-UHFFFAOYSA-L disodium;phenyl phosphate Chemical compound [Na+].[Na+].[O-]P([O-])(=O)OC1=CC=CC=C1 TYJOJLOWRIQYQM-UHFFFAOYSA-L 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- 229940079593 drug Drugs 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000004140 cleaning Methods 0.000 abstract 2
- 238000000151 deposition Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000004128 high performance liquid chromatography Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000470 constituent Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 208000003251 Pruritus Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- 241001013934 Erigeron breviscapus Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- AFEMMXLADCRCSV-UHFFFAOYSA-N benzene;phosphoric acid;sodium Chemical compound [Na].[Na].OP(O)(O)=O.C1=CC=CC=C1 AFEMMXLADCRCSV-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- QCAWEPFNJXQPAN-UHFFFAOYSA-N methoxyfenozide Chemical compound COC1=CC=CC(C(=O)NN(C(=O)C=2C=C(C)C=C(C)C=2)C(C)(C)C)=C1C QCAWEPFNJXQPAN-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000011003 system suitability test Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Images
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- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Description
峰号 | 峰名 | 保留时间 | 峰高 | 峰面积 | 含量 |
1234 | 4.1489.83213.23215.648 | 25.44469.07338.41221125.418 | 310.6001558.100933.300674148.813 | 0.04590.23020.137999.5861 | |
总计 | 21258.347 | 676950.812 | 100.0000 |
峰宽 | 斜率 | 漂移 | 最小面积 | 时间变参 | 锁定时间 | 停止时间 | 样品重量 |
10 | 17.822 | 0.000 | 10.000 | 0.000 | 4.000 | 40.090 | 0.0000 |
Claims (6)
Priority Applications (1)
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---|---|---|---|
CNB2005100107230A CN100352826C (zh) | 2005-04-01 | 2005-04-01 | 高纯度灯盏花乙素原料药的制备工艺 |
Applications Claiming Priority (1)
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CNB2005100107230A CN100352826C (zh) | 2005-04-01 | 2005-04-01 | 高纯度灯盏花乙素原料药的制备工艺 |
Publications (2)
Publication Number | Publication Date |
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CN1840537A true CN1840537A (zh) | 2006-10-04 |
CN100352826C CN100352826C (zh) | 2007-12-05 |
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CNB2005100107230A Active CN100352826C (zh) | 2005-04-01 | 2005-04-01 | 高纯度灯盏花乙素原料药的制备工艺 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102225958A (zh) * | 2011-05-27 | 2011-10-26 | 浙江大学 | 一种野黄芩苷的纯化方法 |
CN102659875A (zh) * | 2012-04-27 | 2012-09-12 | 段志雄 | 一种灯盏花素的提取方法 |
CN101747395B (zh) * | 2009-12-25 | 2013-01-30 | 中国医药集团总公司四川抗菌素工业研究所 | 一种高纯度灯盏花素乙素的制备方法 |
WO2013155849A1 (zh) * | 2012-04-18 | 2013-10-24 | 昆明制药集团股份有限公司 | 一种制备5,6,4'-三羟基黄酮-7-0-d-葡萄糖醛酸的方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1053609A (zh) * | 1990-01-25 | 1991-08-07 | 云南省生物制药厂 | 灯盏花素片剂原料药的提取工艺 |
-
2005
- 2005-04-01 CN CNB2005100107230A patent/CN100352826C/zh active Active
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101747395B (zh) * | 2009-12-25 | 2013-01-30 | 中国医药集团总公司四川抗菌素工业研究所 | 一种高纯度灯盏花素乙素的制备方法 |
CN102225958A (zh) * | 2011-05-27 | 2011-10-26 | 浙江大学 | 一种野黄芩苷的纯化方法 |
WO2013155849A1 (zh) * | 2012-04-18 | 2013-10-24 | 昆明制药集团股份有限公司 | 一种制备5,6,4'-三羟基黄酮-7-0-d-葡萄糖醛酸的方法 |
CN102659875A (zh) * | 2012-04-27 | 2012-09-12 | 段志雄 | 一种灯盏花素的提取方法 |
CN102659875B (zh) * | 2012-04-27 | 2014-12-10 | 段志雄 | 一种灯盏花素的提取方法 |
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Publication number | Publication date |
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CN100352826C (zh) | 2007-12-05 |
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EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Beijing Chuangli-Kechuang Pharmacy Technology Development Co., Ltd. Assignor: Fan Xiane Contract fulfillment period: 2009.4.8 to 2025.3.31 Contract record no.: 2009990000566 Denomination of invention: Process for preparing high-purity scutellarin bulk drug Granted publication date: 20071205 License type: Exclusive license Record date: 20090527 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.4.8 TO 2025.3.31; CHANGE OF CONTRACT Name of requester: BEIJING CHUANGLI KECHUANG MEDICINE TECHNOLOGY DEVE Effective date: 20090527 |
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Owner name: KUNMING LONGJIN PHARMACEUTICAL CO.,LTD Free format text: FORMER OWNER: FAN XIANE Effective date: 20100512 |
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Free format text: CORRECT: ADDRESS; FROM: 650228 KUNMING LONGJIN PHARMACEUTICAL CO., LTD.,WUJIADUI, XIADUAN,XINWEN ROAD,KUNMING CITY,YUNNAN PROVINCE TO: 650106 NO.2188, KEGAO ROAD, KUNMING CITY HIGH-TECH ZONE, YUNNAN PROVINCE |
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Effective date of registration: 20100512 Address after: 650106 No. 2188 Gao Lu, hi tech Zone, Yunnan, Kunming Patentee after: Kunming Longjin Pharmaceutical Co., Ltd. Address before: 650228, Yunnan City, Kunming province road under the five pile of Kunming Long Jin Pharmaceutical Co., Ltd. Patentee before: Fan Xiane |
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CP02 | Change in the address of a patent holder |
Address after: 650500 No. 789, Lanmao Road, majinpu sub district office, Kunming high tech Zone, Kunming, Yunnan Patentee after: KUNMING LONGJIN PHARMACEUTICAL Co.,Ltd. Address before: 650106 No. 2188 Kegao Road, high tech Zone, Kunming, Yunnan Patentee before: KUNMING LONGJIN PHARMACEUTICAL Co.,Ltd. |
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