CN1210289C - 两头尖提取物的制备工艺和用途 - Google Patents
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Abstract
本发明公开一种两头尖提取物的制备工艺和用途，从两头尖及其茎、叶、花、果中提取具有药用价值的总皂甙及单体皂甙D，适用于工业化生产，并制成药物，用于治疗恶性肿瘤疾病。两头尖活性成分的提取分离和鉴定，阐明了两头尖功能主治的物质基础，两头尖总皂甙具有极明显的抗癌活性，对小鼠体内Hep-A-22肝癌的抑瘤率为79%，对C57小鼠Lewis肺癌的抑瘤率为71%。在体外能显著抑制小鼠S180和腹水型肝细胞的DNA、RNA和蛋白质合成，其抑制率随剂量的增多和时间的延长而增加。其抗癌机理主要是由于抑制癌细胞的DNA合成。
Description
本发明公开一种两头尖提取物的制备工艺和用途，涉及中药有效成分的提取制备工艺技术和用途领域。
两头尖为毛莨科银莲花属植物多被银莲花(Anemone raddeanaRegel)的干燥根茎，作为中药在中医临床上具有“祛风湿、消痈肿”的作用，用于“风寒湿痹、四肢拘挛、骨节疼痛、痈肿溃烂”，现代药学研究表明两头尖及其茎、叶、花、果中的总皂甙具有消炎、镇痛、镇静、抑菌等生物活性，特别是皂甙D的上述活性较强，目前，上述物质的提取分离只局限于实验室研究阶段，无法达到工业化生产和开发新药用途。
本发明提供一种两头尖提取物的制备工艺，目的旨在从两头尖中提取具有药用价值的总皂甙及单体皂甙D，适用于工业化生产。
本发明的另一目的是提供两头尖总皂甙及皂甙D制成的药物，用于治疗恶性肿瘤。
本发明的进一步目的是提供上述提取物在制备治疗恶性肿瘤的药物方面的用途。
本发明的技术解决方案包括以下步骤：
1、取两头尖及其茎、叶、花、果粉碎成20目左右粗粉；
2、加5～9倍量的50～70％乙醇进行提取，或用水煎醇沉法提取，过滤并回收乙醇；
3、经大孔吸附树脂吸附，除去色素、糖类等，再用水洗脱树脂至无色，也可用碱溶液洗脱，柱中即为皂甙部分；
4、用50％～70％的乙醇进行洗脱，回收乙醇至无醇味，加入适量的明胶，过滤，上脱色大孔树脂，用50％～70％乙醇洗脱，回收乙醇，浓缩干燥，获得两头尖总皂甙；
5、将两头尖总皂甙用甲醇溶解，上硅胶干柱层析分离，洗脱至柱底，洗脱液为氯仿∶甲醇∶水＝75～55∶45～25∶20～1；
6、收集柱中含皂甙D硅胶，用甲醇洗脱至无皂甙反应，回收甲醇至干，通过醇重结晶，得到无色粉末状结晶两头尖皂甙D。
取两头尖总皂甙干粉加适量淀粉，以70％乙醇制粒，干燥分装制成口服胶囊。
称取两头尖皂甙D10份、氯化钠75份，加蒸馏水适量，用1～5％的氢氧化钠溶液调PH7.5～8.5，加蒸馏水10000ml，经过滤，在无菌条件下灌装和冷冻干燥，制成注射用皂甙D粉针。
本发明的药物含有治疗有效量的提取物为活性成分，以及含有一种或多种药学上可接受的载体。
本发明的提取物可用于制备治疗癌症，特别是肝癌、胃腺癌、肺癌、乳腺癌等癌症的药物。
上文的载体是指药学领域常规的药物载体，包括稀释剂、赋形剂，填充剂，粘合剂，湿润剂，崩解剂，吸收促进剂，表面活性剂，吸附载体等。
本发明可以组合物的形式通过口服、直肠、静脉、肌肉注射或外用给药方式施用于这种治疗的患者。按照药学领域的常规生产方法制备各种剂型如片剂、颗粒剂、冲剂、胶囊、栓剂、喷雾剂、缓释剂和注射剂等。也可使其活性成分与一种或多种载体或药物混合，制成所需剂型。
本发明的药物组合物优选重量比为0.1％～99.5％活性成分。
本发明的施药量可根据用药途径、患者年龄、体重、疾病类型和严重程度等变化，日剂量为0.01～20mg/kg。
两头尖活性成分的提取分离和鉴定，阐明了两头尖功能主治的物质基础，本发明人发现两头尖总皂甙具有极明显的抗癌活性，对小鼠体内Hep-A-22肝癌的抑瘤率为79％，对C57小鼠Lewis肺癌的抑瘤率为71％。体外能显著抑制小鼠S180和腹水型肝细胞的DNA、RNA和蛋白质合成，其抑制率随剂量的增多和时间的延长而增加。其抗癌机理主要是由于抑制癌细胞的DNA合成。
下面的实施例可使本领域的技术人员更全面理解本发明，但不以任何形式限制本发明。
实施例1
两头尖总皂甙的制备
取两头尖包括茎、叶、花、果10公斤，粉碎成20目粗粉，加50公斤的70％乙醇，回流提取3次，每次2小时，过滤提取液合并，减压回收乙醇至无醇味，经喷雾干燥成干粉，加入70％的乙醇溶解，上D101大孔吸附树脂柱，用水洗至无色后，用70％的乙醇洗脱至无皂甙反应为止，将洗脱液用1％活性炭脱色30分钟，趁热过滤，回收乙醇至无醇味，喷雾干燥成细粉，得黄褐色粉末0.5公斤。
实施例2
两头尖总皂甙的制备
取两头尖10公斤，粉碎成20目粗粉，加100公斤的水煎煮三次，每次2小时，合并煎液，过滤，滤液浓缩至相对密度为1.18～1.20(80℃～85℃热测)，加乙醇，使乙醇含量达70％，静止24小时，过滤，回收乙醇，至小体积，加乙醇使醇含量达90％，静止24小时，过滤，滤液回收乙醇至无醇味，喷雾干燥，得黄褐色粉末。
实施例3
两头尖皂甙D的制备
取两头尖粗粉100克，加70％乙醇500ml渗漉至无皂甙反应，回收乙醇至无醇味，经减压干燥并粉碎成干膏粉，加入甲醇溶解，拌如入5倍量的硅胶，上硅胶柱，样品∶硅胶＝1∶150进行干柱层析，用氯仿∶甲醇∶水＝65∶25∶5配成的洗脱液洗脱至柱底，取硅胶切割成段，用甲醇洗脱，薄层析鉴定，收集皂甙D部分，继续用甲醇洗脱至无皂甙反应，减压回收甲醇至干，用乙醇重结晶，得无色粉末状晶体。
实施例4
胶囊：两头尖总皂甙 2500克
玉米淀粉 500克
制备方法：将两头尖总皂甙与玉米淀粉混合搅拌均匀，加入适量70％乙醇湿润制粒，干燥装入胶囊中，制成胶囊1000粒，每个胶囊0.3克。
实施例5
注射用粉针剂：两头尖皂甙D 15克
氯化纳 75克
注射用水 10000ml
制备过程：将两头尖皂甙D、氯化钠溶解于适量的注射用蒸馏水中，用1～5％的氢氧化钠溶液调PH8.0，加注射用水至10000ml，通过0.2μm的微孔滤膜过滤所得溶液，在无菌条件下装入安瓶，冷冻干燥。
实施例6
实施例1提取物的抑瘤作用：总皂甙制成的胶囊经药效学研究，能明显抑制肉瘤S180，肝癌、宫颈癌，其抑癌率分别为49％，54％，84％，对离体细胞株增殖的影响试验表明，在药物的直接作用下，对肝癌细胞株，肺腺癌细胞株，胃腺癌细胞株，乳腺癌细胞株的增殖均有抑制作用，其抑制率分别在75％，76％，73％，84％以上。
实施例7
两头尖皂甙D制成的注射用粉针以5-氟尿嘧啶为对照药，对小鼠体内Hep-A-22肝癌的抑瘤率为74％。对C57小鼠Lewis肺癌的抑瘤率为71％。对Bre-04人体乳腺癌，C01-06人体肠癌的抑瘤率在54～41范围。体外100μg/ml对人体肝、肺、乳腺及肠癌细胞毒试验IC50结果均表明具有20μg/ml的细胞毒作用，对乳腺癌细胞更敏感，体外对人体肝癌、人胃腺癌、人肺癌、乳腺癌的抑制率分别为75％、76％、53％、58％。本注射液能抑制前身物(DNA)掺入体外培养的AH细胞，特别是对S180细胞3H-TdR掺入DNA合成有显著的抑制作用。
Claims (2)
1、一种两头尖提取物的制备工艺，其特征在于包括以下工艺步骤获得：
1)两头尖及其茎、叶、花、果粉碎成20目左右粗粉；
2)加5～9倍的50～70％乙醇进行提取，或用水煎醇沉法提取，过滤并回收乙醇；
3)经大孔吸附树脂吸附，除去色素、糖类，再用水洗脱树脂至无色，柱中即为皂甙部分；
4)用50～70％的乙醇进行洗脱，回收乙醇至无醇味，加入适量的明胶，过滤，上脱色大孔树脂柱，用50～70％乙醇洗脱，回收乙醇，浓缩干燥，获得两头尖总皂甙；
5)将两头尖总皂甙用甲醇溶解，上硅胶干柱层析分离，洗脱至柱底，洗脱液为氯仿∶甲醇∶水＝75～55∶45～25∶20～1；
6)收集柱中硅胶，用甲醇洗脱至无皂甙反应，回收甲醇至干，通过醇重结晶，得到无色粉末结晶两头尖皂甙D。
2、权利要求1所得的提取物在制备治疗肺癌、胃腺癌、乳腺癌药物中的用途。
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011060867A CN1210289C (zh) | 2001-01-16 | 2001-01-16 | 两头尖提取物的制备工艺和用途 |
| US10/466,287 US20040067263A1 (en) | 2001-01-16 | 2002-01-16 | Method for preparating an anemone raddeana extract and the pharmaceutical composition containing the same as well as use thereof |
| JP2002567328A JP2004518751A (ja) | 2001-01-16 | 2002-01-16 | Ｌｉａｎｇｔｏｕｊｉａｎ抽出物の製造方法、その抽出物を含有する医薬組成物及びその用途 |
| PCT/CN2002/000020 WO2002067962A1 (fr) | 2001-01-16 | 2002-01-16 | Procede de preparation d'un extrait d'anemone raddeana, composition pharmaceutique contenant ledit extrait et utilisation d'une telle composition pharmaceutique |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB011060867A CN1210289C (zh) | 2001-01-16 | 2001-01-16 | 两头尖提取物的制备工艺和用途 |
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| Publication Number | Publication Date |
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| CN1312253A CN1312253A (zh) | 2001-09-12 |
| CN1210289C true CN1210289C (zh) | 2005-07-13 |
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| Country | Link |
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| US (1) | US20040067263A1 (zh) |
| JP (1) | JP2004518751A (zh) |
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| WO (1) | WO2002067962A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1312170C (zh) * | 2002-12-27 | 2007-04-25 | 成都和康药业有限责任公司 | 一种两头尖提取物的制备工艺及其提取物在制备治疗癌症的药物中的应用 |
| CN1329037C (zh) * | 2003-05-07 | 2007-08-01 | 丽珠集团利民制药厂 | 一种三七总皂苷静脉注射液及其生产方法 |
| WO2005002609A1 (en) * | 2003-07-01 | 2005-01-13 | Max Zeller Söhne Ag | Plant extraction method and extract |
| US7744929B2 (en) * | 2003-09-15 | 2010-06-29 | Ambotan Pharma, Llc | Botanical drug compositions for treatments of liver and immunological disorders |
| CN101062045B (zh) * | 2006-04-29 | 2011-06-22 | 华北制药集团新药研究开发有限责任公司 | 一类三萜皂苷化合物在制备肿瘤药物中的用途 |
| US20090041618A1 (en) * | 2007-08-06 | 2009-02-12 | Case Medical Inc. | Reusable porous metal filter |
| US8217165B2 (en) * | 2008-06-17 | 2012-07-10 | Pawan Kumar Goel | Process for the extraction of furostanolic saponins from fenugreek seeds |
| CN101492489B (zh) * | 2009-03-06 | 2011-12-07 | 吉林大学 | 银莲花素a的提取方法及其脂微球制剂的制备方法 |
| CN102649807A (zh) * | 2011-02-25 | 2012-08-29 | 苏州宝泽堂医药科技有限公司 | 一种狗哇花皂苷(ⅰ)的制备方法 |
| CN102351922A (zh) * | 2011-08-04 | 2012-02-15 | 浙江工业大学 | 一种从油茶枯饼中提取茶皂素的方法 |
| CN105616552B (zh) * | 2014-11-28 | 2019-10-15 | 天津耀宇生物技术有限公司 | 两头尖提取物的制备方法及其应用 |
| CN105641078B (zh) * | 2014-11-28 | 2019-09-17 | 天津耀宇生物技术有限公司 | 从两头尖中提取活性组分的方法及其应用 |
| KR102118433B1 (ko) | 2018-05-04 | 2020-06-03 | 백주연 | 항암성 사포닌을 고농도로 함유하는 꿩의 바람꽃, 인동속 식물 및 두릅 추출물을 포함하는 암 예방 또는 치료용 조성물 및 이의 제조 방법 |
| KR102529752B1 (ko) * | 2020-06-05 | 2023-05-11 | 김숭진 | 백두옹(Pulsatilla koreana)과 꿩의바람꽃(Anemone raddeana)의 가수분해추출물을 유효성분으로 포함하는 염증성질환 예방 또는 치료용 조성물 |
| KR20240150862A (ko) * | 2023-04-10 | 2024-10-17 | 충남대학교산학협력단 | 항암성 사포닌을 고농도로 함유하는 꿩의바람꽃 추출물의 제조방법 |
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| CN1044561C (zh) * | 1991-10-05 | 1999-08-11 | 邱兴军 | 一种治疗癌症的组合物的制作方法 |
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- 2002-01-16 JP JP2002567328A patent/JP2004518751A/ja active Pending
- 2002-01-16 WO PCT/CN2002/000020 patent/WO2002067962A1/zh not_active Ceased
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| Publication number | Publication date |
|---|---|
| WO2002067962A1 (fr) | 2002-09-06 |
| US20040067263A1 (en) | 2004-04-08 |
| JP2004518751A (ja) | 2004-06-24 |
| CN1312253A (zh) | 2001-09-12 |
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