CN105601700B - 从雷公藤中制备雷公藤乙素的方法 - Google Patents
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- YKUJZZHGTWVWHA-UHFFFAOYSA-N triptolide Natural products COC12CC3OC3(C(C)C)C(O)C14OC4CC5C6=C(CCC25C)C(=O)OC6 YKUJZZHGTWVWHA-UHFFFAOYSA-N 0.000 title claims abstract description 55
- DFBIRQPKNDILPW-CIVMWXNOSA-N Triptolide Chemical compound O=C1OCC([C@@H]2C3)=C1CC[C@]2(C)[C@]12O[C@H]1[C@@H]1O[C@]1(C(C)C)[C@@H](O)[C@]21[C@H]3O1 DFBIRQPKNDILPW-CIVMWXNOSA-N 0.000 title claims abstract description 54
- 241000830536 Tripterygium wilfordii Species 0.000 title claims abstract description 24
- 235000015398 thunder god vine Nutrition 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 93
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 19
- 239000000284 extract Substances 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 16
- 239000000499 gel Substances 0.000 claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 239000000741 silica gel Substances 0.000 claims abstract description 11
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 11
- 239000002024 ethyl acetate extract Substances 0.000 claims abstract description 9
- 241000545405 Tripterygium Species 0.000 claims abstract description 8
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 239000003480 eluent Substances 0.000 claims description 30
- 238000010828 elution Methods 0.000 claims description 28
- 239000003208 petroleum Substances 0.000 claims description 15
- SRCZQMGIVIYBBJ-UHFFFAOYSA-N ethoxyethane;ethyl acetate Chemical compound CCOCC.CCOC(C)=O SRCZQMGIVIYBBJ-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 10
- 238000004440 column chromatography Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 5
- UREBWPXBXRYXRJ-UHFFFAOYSA-N ethyl acetate;methanol Chemical compound OC.CCOC(C)=O UREBWPXBXRYXRJ-UHFFFAOYSA-N 0.000 claims description 5
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J73/00—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms
- C07J73/001—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by one hetero atom
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Abstract
本发明公开了一种从雷公藤中制备雷公藤乙素的方法。将雷公藤根用乙醇水溶液加热回流提取,得到总浸膏。将总浸膏用乙酸乙酯溶解数次至不再溶解,得乙酸乙酯部位。将乙酸乙酯部位依次经中性氧化铝色谱柱、MCI GEL色谱柱和硅胶色谱柱层析,得雷公藤乙素粗品。最后用乙酸乙酯重结晶,得雷公藤乙素纯品。该法提取制备过程相对简单、设备要求低、产品得率高、纯度高、适合雷公藤乙素的大规模分离制备。
Description
技术领域
本发明属于药物制备领域,特别涉及一种从雷公藤中制备雷公藤乙素的方法。
背景技术
雷公藤( Tripteryginum Wilfordii Hook. F) 又名黄藤、黄藤木、黄腊藤、黄檀根、断肠草等,属卫茅科植物。味辛、苦,性凉,有大毒,归心、肝、脾、肾经,有清热解毒,祛风除湿,舒筋活血通络,消肿止痛,杀虫止痒之功。主要分布福建、湖南、江西等地。临床常用于治疗类风湿性关节炎、慢性肾炎、红斑狼疮等难治性免疫功能亢进疾病。目前有雷公藤片、雷公藤多苷片、雷公藤内酯、雷公藤内酯软膏、雷公藤总萜片等国家药品标准收载的多个国产药品品种广泛应用于临床,疗效显著。
雷公藤乙素(Tripdiolide),又名雷公藤内酯二醇,是雷公藤中的一种二萜内酯类成分。雷公藤乙素是雷公藤的主要活性成分,也是雷公藤多苷片和雷公藤总萜片的主要有效成分。研究表明雷公藤乙素具有抗炎、免疫抑制、抗肿瘤以及治疗糖尿病肾病等作用,具有很好的药用开发前景。
目前关于雷公藤乙素的制备方法有:雷公藤提取物反复柱层析制备法,雷公藤提取物高效液相色谱制备法,雷公藤提取物高速逆流色谱制备法等。这些方法有的过程非常复杂、提取制备效率低,有的产品纯度不高、得率低,有的需要昂贵仪器设备、有机溶剂的用量很大、成本高、难以适合雷公藤乙素的大规模分离制备。
本发明公开了一种从雷公藤中制备雷公藤乙素的方法,该法与现有方法比较,具有提取制备过程相对简单、设备要求低、产品得率高、纯度高、适合雷公藤乙素的大规模分离制备等优势。
发明内容
本发明的目的是提供一种从雷公藤中制备雷公藤乙素的方法,该法与现有方法比较,具有提取制备过程相对简单、设备要求低、产品得率高、纯度高、适合雷公藤乙素的大规模分离制备等优势。
本发明的技术方案如下:
(1)将雷公藤根切片,用3~10倍量的乙醇水溶液(70%~95%)加热回流提取3次,每次1.5小时,合并提取液,减压浓缩回收乙醇得到总浸膏。将总浸膏用乙酸乙酯溶解数次至不再溶解,合并乙酸乙酯溶液,减压浓缩回收乙酸乙酯得乙酸乙酯部位。
(2)将乙酸乙酯部位经10~30倍量中性氧化铝色谱柱层析,先用石油醚—乙酸乙酯(2:3,V/V)洗脱,洗脱液弃去,再用乙酸乙酯—甲醇(3:1,V/V)洗脱,收集洗脱液,减压浓缩得中性氧化铝色谱柱洗脱部位。
(3)将中性氧化铝色谱柱洗脱部位经MCI GEL色谱柱层析,先用甲醇—水(1:3,V/V)洗脱,洗脱液弃去,再用甲醇—水(1:1,V/V)洗脱,收集洗脱液,减压浓缩得MCI GEL色谱柱洗脱部位。
(4)将MCI GEL色谱柱洗脱部位经10~30倍量硅胶色谱柱层析,先用石油醚—乙酸乙酯(7:4,V/V)洗脱,洗脱液弃去,再用石油醚—乙酸乙酯(1:1,V/V)洗脱,收集洗脱液,减压浓缩得硅胶色谱柱洗脱部位,并析出雷公藤乙素粗品。
(5)将雷公藤乙素粗品用乙酸乙酯结晶,得到雷公藤乙素粗晶,再用乙酸乙酯重结晶1~2次,得雷公藤乙素纯晶,采用雷公藤乙素对照品对照HPLC法以及核磁共振波谱法鉴定产品。经HPLC检测雷公藤乙素含量大于99%。相对于雷公藤药材中雷公藤乙素的量,该法制得雷公藤乙素产品得率大于90%。
具体实施方式
下面结合实施例对本发明作进一步详细说明,但应理解本发明的范围非仅限于这些实施例的范围。
实施例1:
将雷公藤根30千克切片,用10倍量的95%乙醇水溶液加热回流提取3次,每次1.5小时,合并提取液,减压浓缩回收乙醇得到总浸膏2915克。将总浸膏用乙酸乙酯溶解数次至不再溶解,合并乙酸乙酯溶液,减压浓缩回收乙酸乙酯得乙酸乙酯部位480克。将乙酸乙酯部位经30倍量中性氧化铝色谱柱层析,先用石油醚—乙酸乙酯(2:3,V/V)洗脱,洗脱液弃去,再用乙酸乙酯—甲醇(3:1,V/V)洗脱,收集洗脱液,减压浓缩得中性氧化铝色谱柱洗脱部位36克。将中性氧化铝色谱柱洗脱部位经MCI GEL色谱柱层析,先用甲醇—水(1:3,V/V)洗脱,洗脱液弃去,再用甲醇—水(1:1,V/V)洗脱,收集洗脱液,减压浓缩得MCI GEL色谱柱洗脱部位3.3克。将MCI GEL色谱柱洗脱部位经30倍量硅胶色谱柱层析,先用石油醚—乙酸乙酯(7:4,V/V)洗脱,洗脱液弃去,再用石油醚—乙酸乙酯(1:1,V/V)洗脱,收集洗脱液,减压浓缩得硅胶色谱柱洗脱部位,并析出雷公藤乙素粗品0.12克。将雷公藤乙素粗品用乙酸乙酯结晶,得到雷公藤乙素粗晶,再用乙酸乙酯重结晶1次,得雷公藤乙素纯晶0.084克,采用雷公藤乙素对照品对照HPLC法以及核磁共振波谱法鉴定产品。经HPLC检测雷公藤乙素含量为99.1%。经HPLC测得雷公藤药材中雷公藤乙素含量为3.1ppm。相对于雷公藤药材中雷公藤乙素的量,雷公藤乙素产品得率为90.3%。
实施例2:
将雷公藤根30千克切片,用3倍量的70%乙醇水溶液加热回流提取3次,每次1.5小时,合并提取液,减压浓缩回收乙醇得到总浸膏3045克。将总浸膏用乙酸乙酯溶解数次至不再溶解,合并乙酸乙酯溶液,减压浓缩回收乙酸乙酯得乙酸乙酯部位498克。将乙酸乙酯部位经10倍量中性氧化铝色谱柱层析,先用石油醚—乙酸乙酯(2:3,V/V)洗脱,洗脱液弃去,再用乙酸乙酯—甲醇(3:1,V/V)洗脱,收集洗脱液,减压浓缩得中性氧化铝色谱柱洗脱部位38克。将中性氧化铝色谱柱洗脱部位经MCI GEL色谱柱层析,先用甲醇—水(1:3,V/V)洗脱,洗脱液弃去,再用甲醇—水(1:1,V/V)洗脱,收集洗脱液,减压浓缩得MCI GEL色谱柱洗脱部位4.1克。将MCI GEL色谱柱洗脱部位经10倍量硅胶色谱柱层析,先用石油醚—乙酸乙酯(7:4,V/V)洗脱,洗脱液弃去,再用石油醚—乙酸乙酯(1:1,V/V)洗脱,收集洗脱液,减压浓缩得硅胶色谱柱洗脱部位,并析出雷公藤乙素粗品0.13克。将雷公藤乙素粗品用乙酸乙酯结晶,得到雷公藤乙素粗晶,再用乙酸乙酯重结晶2次,得雷公藤乙素纯晶0.085克,采用雷公藤乙素对照品对照HPLC法以及核磁共振波谱法鉴定产品。经HPLC检测雷公藤乙素含量为99.2%。经HPLC测得雷公藤药材中雷公藤乙素含量为3.1ppm。相对于雷公藤药材中雷公藤乙素的量,雷公藤乙素产品得率为91.3%。
实施例3:
将雷公藤根30千克切片,用6倍量的85%乙醇水溶液加热回流提取3次,每次1.5小时,合并提取液,减压浓缩回收乙醇得到总浸膏3002克。将总浸膏用乙酸乙酯溶解数次至不再溶解,合并乙酸乙酯溶液,减压浓缩回收乙酸乙酯得乙酸乙酯部位496克。将乙酸乙酯部位经20倍量中性氧化铝色谱柱层析,先用石油醚—乙酸乙酯(2:3,V/V)洗脱,洗脱液弃去,再用乙酸乙酯—甲醇(3:1,V/V)洗脱,收集洗脱液,减压浓缩得中性氧化铝色谱柱洗脱部位40克。将中性氧化铝色谱柱洗脱部位经MCI GEL色谱柱层析,先用甲醇—水(1:3,V/V)洗脱,洗脱液弃去,再用甲醇—水(1:1,V/V)洗脱,收集洗脱液,减压浓缩得MCI GEL色谱柱洗脱部位4.3克。将MCI GEL色谱柱洗脱部位经20倍量硅胶色谱柱层析,先用石油醚—乙酸乙酯(7:4,V/V)洗脱,洗脱液弃去,再用石油醚—乙酸乙酯(1:1,V/V)洗脱,收集洗脱液,减压浓缩得硅胶色谱柱洗脱部位,并析出雷公藤乙素粗品0.14克。将雷公藤乙素粗品用乙酸乙酯结晶,得到雷公藤乙素粗晶,再用乙酸乙酯重结晶2次,得雷公藤乙素纯晶0.0841克,采用雷公藤乙素对照品对照HPLC法以及核磁共振波谱法鉴定产品。经HPLC检测雷公藤乙素含量为99.2%。经HPLC测得雷公藤药材中雷公藤乙素含量为3.1ppm。相对于雷公藤药材中雷公藤乙素的量,雷公藤乙素产品得率为90.4%。
Claims (1)
1.从雷公藤中制备雷公藤乙素的方法,其特征在于它包含以下步骤:
① 将雷公藤根切片,用3~10倍量的70%~95%乙醇水溶液加热回流提取3次,每次1.5小时,合并提取液,减压浓缩回收乙醇得到总浸膏,将总浸膏用乙酸乙酯溶解数次至不再溶解,合并乙酸乙酯溶液,减压浓缩回收乙酸乙酯得乙酸乙酯部位;
② 将乙酸乙酯部位经10~30倍量中性氧化铝色谱柱层析,先用体积比2:3的石油醚—乙酸乙酯洗脱,洗脱液弃去,再用体积比3:1的乙酸乙酯—甲醇洗脱,收集洗脱液,减压浓缩得中性氧化铝色谱柱洗脱部位;
③ 将中性氧化铝色谱柱洗脱部位经MCI GEL色谱柱层析,先用体积比1:3的甲醇—水洗脱,洗脱液弃去,再用体积比1:1的甲醇—水洗脱,收集洗脱液,减压浓缩得MCI GEL色谱柱洗脱部位;
④ 将MCI GEL色谱柱洗脱部位经10~30倍量硅胶色谱柱层析,先用体积比7:4的石油醚—乙酸乙酯洗脱,洗脱液弃去,再用体积比1:1的石油醚—乙酸乙酯洗脱,收集洗脱液,减压浓缩得硅胶色谱柱洗脱部位,并析出雷公藤乙素粗品;
⑤ 将雷公藤乙素粗品用乙酸乙酯结晶,得到雷公藤乙素粗晶,再用乙酸乙酯重结晶1~2次,得雷公藤乙素纯晶。
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