CN1219545C - 头花蓼提取物及其药物组合物制剂 - Google Patents
头花蓼提取物及其药物组合物制剂 Download PDFInfo
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Abstract
本发明涉及头花蓼鲜品或干品提取物及其药物组合物制剂。本发明用水、75%乙醇和95%乙醇和二氧化碳超临界萃取方法分别对头花蓼全草、地上部分、叶、种子、茎和根部分别进行了提取和活性研究，本发明工艺得到的头花蓼提取物及其药物组合物制剂如片剂在抗菌、抗炎、镇痛、利尿、治疗肾盂肾炎、前列腺炎和排石等方面具有明显的效果。
Description
技术领域
本发明涉及中药领域，具体而言，本发明涉及中草药头花蓼鲜品或干品的提取物及其制备方法以及这种提取物作为药物的用途。
背景技术
头花蓼(Polygonum capitatum Buch.-Ham.ex D.Don)是蓼科蓼属植物，为多年生草本，别名四季红、石莽草、石辣蓼、水绣球、红花地丁、满地红等。在中国贵州、云南、广西、四川、西藏、湖北、湖南和江西等地区均有分布，主要生长在山坡、山谷及富含煤层的沙页岩地带。全草具有清热解毒、散瘀、利尿通淋之功效。据1963年《广西中药志》第二册记载，头花蓼主要用于治疗风湿痛；1977年《中药大辞典》上册记载，头花蓼主要用于治疗痢疾、肾炎、膀胱炎和尿路结石等。民间一般将头花蓼用水煎服，治疗效果比较明显，但是服用不方便。中国专利申请公开说明书CN1054899A中公开了一种泌感灵冲剂、糖浆生产工艺。该生产工艺包括煎煮、浓缩、提取、再浓缩等步骤，工艺复杂，而且，该方法得到的泌感灵冲剂的药效学效果有待提高。贵州威门药业股份有限公司长期致力于中草药头花蓼的开发利用研究，我们将头花蓼加水煎煮两次后过滤浓缩制成热淋清颗粒，该制剂公开在中华人民共和国卫生部药典委员会1998年编的中华人民共和国卫生部《药品标准--中药成方制剂》(第十七册)中，但是，随着研究的不断深入，本发明人发现，结合药理学试验验证，通过改进提取和精制工艺，本发明人得到的头花蓼提取物的药理活性明显提高，并发现这种头花蓼提取物具有新的疗效，因此完成了本发明。
发明内容
因此，本发明的目的是提供了一种头花蓼鲜品或干品的提取物；
本发明的另一发明目的是提供了一种制备头花蓼提取物的方法；
本发明的另一发明目的是提供了头花蓼提取物用于制备抗菌、抗炎、镇痛、利尿、治疗泌尿系统结石、治疗肾盂肾炎以及前列腺炎的药物的用途；
本发明的另一发明目的是提供了含有本发明提取物的药物组合物。
本发明的目的是通过下列方法实现的。
本发明人分别对头花蓼鲜品或干品的不同药用部位进行了研究，对头花蓼全草、头花蓼地上部分、叶、种子、茎和根部及它们的组合分别进行了提取和活性研究，本发明人发现，头花蓼的叶、种子、茎和根部分的生物学活性是有差别的，抗炎活性以叶提取物为最佳；抗菌活性的强弱顺序是种子＞叶＞茎＞根。本发明人从这一发现中得到启示，用头花蓼的地上部分代替传统使用的头花蓼全草进行提取，这样既保持和提高了提取浸膏的药学活性，又避免使用头花蓼的根部。由于头花蓼是草本植物，不使用其根部，可以避免在采集头花蓼时将其根部拔起，这样，头花蓼可以再生，既保护了植物资源，又保护了土地植被，这对保护资源和环境都有重要意义。
本发明的头花蓼提取物由下列方法制备得到：a.由头花蓼全草的鲜品或干品用水分两次煎煮或用醇水混合液分二至三次回流提取，每次1-2小时，合并煎煮液或提取液，过滤浓缩至20℃时的相对密度为1.2，喷雾干燥或减压干燥得到；或者b.由头花蓼全草或其水提药渣经二氧化碳超临界萃取得到。
本发明人用水、75％乙醇和95％乙醇和二氧化碳超临界条件分别对头花蓼全草、地上部分、叶、种子、茎和根部分别进行了提取和活性研究。
本发明的头花蓼地上部分包括头花蓼茎、叶、花、和/或种子或者它们的混合物；也可以是叶、花和茎；或者是叶、种子和茎；或者是叶和茎等。
本发明的头花蓼提取物是通过下列方法得到的：
具体实施方式
实施例1：制备头花蓼地上部分水提取物(编号：w-2-1)
取头花蓼地上部分220kg，洗净，加入7倍量水，加热煮沸1.5小时，过滤，药渣中加入6倍量水，煮沸1.0小时，过滤。合并滤液，浓缩至相对密度为1.2(20℃)得到浸膏，喷雾干燥得到浸膏粉23kg，收率是10.45％。
采用分光光度计法测定w-2-1中的总黄酮含量，将本发明的方法制备得到的w-2-1提取物和辅料均匀混和，制粒，干燥，即得到新方法制备的热淋清颗粒。
实施例2：制备头花蓼全草水提取物(喷雾干燥)(编号：w-1-2)
根据与实施例1相同的方法，用头花蓼全草代替头花蓼地上部分进行提取。
取w-1-2浸膏粉按实施例1相同的方法，制得样品(w-1-12)。
本发明将头花蓼全草与头花蓼地上部分实验数据进行比较。(见表1)
表1：头花蓼全草水提取物与头花蓼地上部分水提取物实验数据
名称 编号 投料量 得浸膏粉量 收率 没食子酸 总黄酮含量
(kg) (kg) (％) 含量(％) (％)
头花蓼 W-1-2 300.95 34.5 11.46 1.78 1.82
全草
头花蓼 w-2-1 220 23 10.45 3.99 4.71
地上部分
从以上结果看出，以地上部分为原料的浸膏粉中没食子酸和总黄酮含量含量明显高于以全草为原料的浸膏粉。
实施例3：制备头花蓼全草水提取物(减压干燥)(编号：w-1-3)
根据与实施例2相同的方法，将干燥方法改为减压干燥。
实施例4：制备头花蓼根95％乙醇提取物(编号：w-1-4)
取头花蓼根10kg，洗净，置不锈钢浓缩罐内，加入7.5倍量的95％乙醇，回流提取1.5小时，过滤。药渣加入7.5倍量95％乙醇，回流提取1.0小时，过滤。合并两次滤液，浓缩得浸膏，减压干燥得到提取物0.215kg。
实施例5：制备头花蓼茎95％乙醇提取物(编号：w-1-5)
根据与实施例4相同的方法，用头花蓼茎进行提取。
实施例6：制备头花蓼叶95％乙醇提取物(编号：w-1-6)
根据与实施例4相同的方法，用头花蓼叶进行提取。
实施例7：制备头花蓼种子95％乙醇提取物(编号：w-1-7)
根据与实施例4相同的方法，用头花蓼种子进行提取。
实施例8：制备头花蓼鲜品95％乙醇提粉(编号：w-1-8)
根据与实施例4相同的方法，用头花蓼鲜品进行提取。
实施例9：制备头花蓼鲜品水提粉(编号：w-1-9)
根据与实施例3相同的方法，用头花蓼鲜品进行提取。
实施例10：制备头花蓼全草75％乙醇提取物(编号：W-1-10)
取头花蓼全草10kg，洗净，置不锈钢浓缩罐内，加入7-8倍量75％乙醇，回流提取1.5小时，过滤。药渣加入5倍量75％乙醇，回流提取1.0小时，过滤。合并两次滤液，浓缩得浸膏，减压干燥得到提取物0.694kg。
实施例11：制备头花蓼全草水煎醇沉溶液粉(W-1-14a)和头花蓼全草水煎醇沉沉淀粉(W-1-14b)
取头花蓼全草10.60kg，洗净，加入350kg水，加热煮沸1.5小时，转移上清液，残渣中加入150kg水，煮沸1.0小时。合并煎煮液，过滤浓缩至相对密度为1.04(24℃)得浸膏16.1kg。加入95％乙醇调至含醇量为60％，静至24小时，分取溶液。向沉淀加入95％乙醇调至含醇量为60％，静至24小时，分取溶液，合并两次溶液，挥去乙醇，80℃减压干燥得头花蓼全草水煎醇沉溶液粉(W-1-14a)0.755kg；沉淀于80℃减压干燥得头花蓼全草水煎醇沉沉淀粉(W-1-14b)0.465kg。
实施例12：制备头花蓼原药粉二氧化碳超临界萃取提取物(编号：W-1-15a)
取头花蓼原药粉10kg，洗净，投入超临界萃取釜中，对萃取釜和两个解析釜加热，对贮罐进行冷却，当温度达到预定的温度时，打开CO2气瓶送气，当压力达到预定压力时，开始循环萃取，调节流量，并加入夹带剂，恒温恒压萃取2小时。将得到的液体减压浓缩得到浸膏0.135kg。
实施例13：制备头花蓼药渣二氧化碳超临界萃取提取物(编号：W-1-15b)
取头花蓼药渣10kg，洗净，投入超临界萃取釜中，对萃取釜和两个解析釜加热，对贮罐进行冷却，当温度达到预定的温度时，打开CO2气瓶送气，当压力达到预定压力时，开始循环萃取，调节流量，并加入夹带剂，恒温恒压萃取2小时。将得到的液体减压浓缩得到浸膏0.119kg。
实施例14：制备头花蓼地上部分70％乙醇提取物(编号：W-2-2)
取头花蓼地上部分30kg，洗净，置不锈钢浓缩罐内，加入8-9倍量70％乙醇，回流提取1.5小时，过滤。药渣加入4-5倍量70％乙醇，回流提取1.0小时，过滤。药渣再加入4-5倍量70％乙醇，回流提取1.0小时，过滤。合并三次滤液，浓缩得浸膏，减压干燥得到提取物3.75kg。
表2：不同部位、不同提取方法样品的实验数据
| 编号 | 名称 | 投料量(kg) | 得浸膏粉量(kg) | 收率(％) | 没食子酸含量(％) | 总黄酮含量(％) |
| W-1-2W-1-3W-1-4W-1-5W-1-6W-1-7W-1-8W-1-9W-1-10W-1-12W-1-14aW-1-14bW-1-15aW-1-15bW-2-1W-2-2 | 头花蓼全草水提取物(喷雾干燥)头花蓼全草水提取物(减压干燥)根95％乙醇提取物茎95％乙醇提取物叶95％乙醇提取物种子95％乙醇提取物鲜品95％乙醇提粉鲜品水提粉头花蓼全草的75％乙醇提取物W-1-2加辅料制成的颗粒头花蓼全草水煎醇沉溶液粉头花蓼全草水煎醇沉沉淀粉头花蓼原药粉二氧化碳超临界萃取提取物头花蓼药渣二氧化碳超临界萃取提取物头花蓼地上部分水提取物地上部分的70％乙醇提取物 | 300.95300.95101091.8222110/10.6010.60101022030 | 34.532.80.2150.1250.70.030.5500.8550.694/0.7550.4650.1350.119233.75 | 11.4610.902.151.257.781.702.504.076.94/7.124.391.351.1910.4512.5 | 1.782.551.481.890.700.722.872.761.480.733.060.83.995.88 | 1.821.462.251.946.295.553.781.923.171.592.000.644.714.57 |
注：由于样品W-1-15a和样品W-1-15b十分粘稠，前处理很困难，因此没有测定其没食子酸含量和总黄酮含量。
中国发明专利公开说明书CN1054899A中制备头花蓼全草提取物的方法与本文中制备头花蓼全草水煎醇沉溶液粉(W-1-14a)的方法一致。而样品W-1-2实际是全草水煎醇沉溶液粉(W-1-14a)和全草水煎醇沉沉淀粉(W-1-14b)的加和。经过药效学实验证明头花蓼全草水煎醇沉沉淀粉(W-1-14b)同样具有良好的活性；而样品W-1-2则是此三个样品中活性最强的(见表5)。中国发明专利公开说明书CN1054899A中制备头花蓼全草提取物的方法操作烦琐，因经醇沉处理的药液在保存期间容易产生沉淀或粘壁现象；经醇沉回收乙醇后的药液往往粘性较大，较难浓缩。醇沉处理生产周期长，成本高。并且损失掉部分活性成分(即CN1054899A方法中扔掉的水煎醇沉沉淀部分W-1-14b)。
我们对头花蓼全草、地上部分、根、茎、叶、花、种子及地上部分去花(即茎和叶)各部分的水提取物、95％乙醇提取物、CO2超临界提取物都进行了药理学试验，我们发现其中以头花蓼地上部分的疗效最好。并以头花蓼地上部分为原料，用制药领域中的常规方法制成了一系列药物组合物，现成各种制剂：片剂、锭剂、煎膏剂(膏滋)、胶剂、巴布膏剂、合剂、滴丸剂、酒剂、酣剂、流浸膏剂与膏剂、橡胶剂、露剂、茶剂、搽剂、及缓释、控释制剂及靶向制剂。
本发明的各种药物组合物制剂可以根据制药领域中常规的方法，使用制药学上常规的辅料和本发明的提取物制备得到。具体实例如下：
片剂的制备方法：取本发明实施例中制备得到的头花蓼浸膏粉，加辅料适量，混合均匀，制成颗粒，压片，即得。
本发明人将上述提取物进行了药效学研究发现，本发明的头花蓼提取物具有良好的抗菌、抗炎、镇痛、利尿、排石、治疗肾盂肾炎以及前列腺炎等药理学活性。
试验一：抗炎活性研究
实验方法：用小鼠耳部巴豆油炎症模型，根据小鼠耳肿胀生物活性测定法，测定不同药用部位和不同提取工艺得到的提取物的抗炎活性。实验采用小鼠静脉注射给药，给药剂量为40mg/kg，在同等剂量下，比较各提取物样品的抗炎活性大小。以此来对不同药用部位，不同提取工艺样品的疗效作出评判。
样品配制方法：用5％丙二醇作溶媒，将样品称量后，先加入0.5ml丙二醇超声处理，待样品粉末分散均匀后，再用生理盐水稀释至刻度(10ml)。
实验结果：
共进行三批实验，每批实验均在同时相同的实验条件(室温、湿度)下进行。
实验结果见表3
表3 不同头花蓼样品抗炎活性的比较
| 编号 | 名称 | 剂量(mg/kg) | 内含总黄酮量(mg) | 内含没食子酸量(mg) | 第一次实验(n＝10) | 第二次实验(n＝10) | 第三次实验(n＝11) | |||
| 肿胀度(mg) | 肿胀率(％) | 肿胀度(mg) | 肿胀率(％) | 肿胀度(mg) | 肿胀率(％) | |||||
| W-1-2W-1-3W-1-4W-1-5W-1-6阳性对照阳性对照阳性对照 | 全草水提(喷雾)全草水提(减压)根95％醇提茎95％醇提叶95％醇提氢化可的松芦丁没食子酸 | 4040404040202020 | 0.7280.5840.9010.7762.517-20- | 0.8641.0980.5920.4800.305--20 | 13.1±5.0*(30.7)13.1±4.7*(30.7)13.6±4.7*(28.0)14.1±3.5*(25.4)13.0±2.6*(31.2)6.7±2.9**(64.6) | 77.8±36.8*82.6±30.986.1±29.986.4±26.082.1±22.7*45.2±20.7** | 10.8±2.5*(33.7)11.5±2.5**{29.4}12.2±3.2**{25.1}13.9±2.3*(14.7)8.4±3.1**(48.5)4.9±2.8**(69.9)11.4±2.7**(30.1)15.9±3.4(2.4) | 72.2±22.5**75.1±20.3**80.6±19.3**96.2±16.7*57.9±20.4**36.4±16.4**74.7±17.1**107.0±19.5 | 11.5±3.4*(33.1)11.3±2.8**(34.3)14.4±3.1*(16.3)14.5±4.5(15.7)9.8±2.8**(43.0)4.7±1.6**(72.7)11.4±2.9**(33.3)15.3±2.2(11.0) | 64.0±20.2**64.0±17.0**84.7±24.5*80.5±24.7*59.4±17.0**29.7±12.1*65.4±21.3**96.6±18.9 |
| 模型组W-1-2W-1-8W-1-9W-1-15bW-1-15a阳性对照模型组 | 5％丙二醇全草水提鲜品醇提鲜品水提CO2药渣CO2药材氢化可的松5％丙二醇 | 404040404020- | 0.7281.5100.770 | 0.8641.3131.276 | 18.9±5.312.6±3.4**13.0±2.4*(31.2)7.4±2.6**(60.8)12.1±3.3**17.9±2.95.0±2.4**20.4±2.8 | 117.2±43.181.1±26.5**86.2±26.345.8±18.0**77.2±19.2**108.8±29.434.8±18.0124.8±21.1 | 16.3±2.57 3±2.5**13.5±3.0*(17.2)9.5±3.7**(41.7)7.6±1.6**10.4±3.22.4±1.3**13.4±3.3 | 117.8±24.041.7±15.4**85.1±32.2*57.8±29.4**40.7±9.7**57.1±21.913.8±7.8**73.7±20.9 | 17.2±2.87.8±3.4**13.2±3.1*(23.3)8.8±2.8**(48.8)4.1±1.9**7.1±3.9**2.2±1.4**12.5±4.1 | 104.4±16.647.3±22.2**77.3±23.8**55.2±22.8**25.8±12.6**43.8±22.7**13.4±8.682.5±28.9** |
备注：1.氢化可的松、芦丁、没食子酸用生理盐水配制，其余样品用5％丙二醇配制。2.除根醇提粉样品在丙二醇中分散较难而超声4小时外，其余样品均超声10分钟处理。3.“*”“**”分别表示与模型组比较P＜0.05、P＜0.01。从三次实验结果分析得出：
1.喷雾干燥与减压干燥工艺所生产出的样品，从抗炎角度(40mg/kg)来看二者无明显差异。
2.根、茎、叶三醇提样品以叶醇提粉抗炎作用最佳，表明头花蓼抗炎活性成分主要在叶子中间，对三个部位醇提样品的三次试验结果归纳统计处理见表4。
表4 根、茎、叶中黄酮含量与抗炎相关性统计分析
样品编号 名称 黄酮含量 肿胀抑制率 γ值
w-1-4 根醇提粉 22.53 28.0
w-1-4 根醇提粉 22.53 25.1
w-1-4 根醇提粉 22.53 16.3
w-1-5 茎醇提粉 19.41 25.4 γ＝0.850
w-1-5 茎醇提粉 19.41 14.7 P＜0.01
w-1-5 茎醇提粉 19.41 15.7
w-1-6 叶醇提粉 62.93 31.2
w-1-6 叶醇提粉 62.93 48.5
w-1-6 叶醇提粉 62.93 43.0
由此可见：抗炎活性与上述三个部位的黄酮含量有正相关性关系。
3.鲜品醇提和鲜品水提二者比较，水提成分的抗炎作用明显优于醇提成分。表明头花蓼的抗炎作用活性成分主要为水溶性。
4.芦丁、没食子酸剂量均达到20mg/kg，远远超过上述头花蓼样品中的含量。实验结果仅显示出芦丁有抗炎效果，但作用强度未能超过头花蓼提取成分的数倍，说明头花蓼中抗炎成分除黄酮外还有其他活性成分存在，而没食子酸可能不是抗炎成份。
试验结果说明：
1.头花蓼根、茎、叶醇提样品以叶醇提粉抗炎作用最佳，表明头花蓼抗炎活性成分主要在叶子中，去掉根部，头花蓼地上部分的抗炎活性不受影响；
2.水提成分的抗炎作用明显优于醇提成分，表明头花蓼的抗炎作用活性成分主要为水溶性。
试验二：体内外抗菌活性研究
体外抗菌实验方法：采用琼脂二倍稀释法测定不同药用部位和不同提取工艺得到的提取物的最低抑菌浓度(MIC)。用多点接种仪将细菌接种于含不同药物浓度的琼脂平皿表面，每点含菌量约为105CFU/ml，37℃孵育18小时(淋球菌孵育48小时)观察结果，以无细菌生长平皿培养基中所含药物的最低浓度为药物对该菌的最低抑菌浓度(MIC值)。
体内抗菌保护实验方法：将实验动物按性别、体重均匀分组，每组10只小鼠，雌雄各半，给小鼠灌胃不同用药部位、不同提取工艺的头花蓼样品，每日一次，0.5ml/20g鼠重，预先连续灌胃给药3天，于第3天给药后各组小鼠腹腔感染受试菌液，每鼠感染菌量为0.5ml(1MLD)，氟哌酸胶囊于感染菌液后即刻及4小时再灌胃给药一次，同时设感染对照组及药物对照组(不感染菌)，记录感染后七天内小鼠存活数，根据感染后七天动物存活数计算其半数有效剂量(ED50)及其95％可信限或计算感染后七天动物存活数与感染对照组比较的t测验值，判断与感染对照组比较有无差异。
实验结果：
(一)体外抗菌实验结果见表5。
1.没食子酸、种子醇提取物(w-1-7)对所试革兰氏阳性，阴性细菌及白色念珠菌均呈现出一定的抗菌活力，其次是叶醇提取物(w-1-6)、头花蓼75％乙醇提物(w-1-10)、喷雾干燥(w-1-2)和减压干燥(w-1-3)。
2.11 种头花蓼样品对所试临床分离淋球菌具有良好的体外抗菌活性。
3.11 种头花蓼样品对本次试验中临床分离金黄色葡萄球菌、表皮葡萄球菌的抗菌活力强于链球菌。
4.11 种头花蓼样品对本次试验中对所试的阴性杆菌的大肠埃希菌、变形杆菌、痢疾杆菌的MIC范围在1.56～400mg/ml；对肺炎克雷伯杆菌和铜绿假单胞菌的MIC范围为6.25～＞40mg/ml.
5.11 种头花蓼样品对白色念珠菌的抗菌活力较弱。
6.头花蓼喷雾干燥粉(W-1-2)对皮肤真菌如石膏样小孢子菌、石膏癣菌，红色毛癣菌的MIC值为25～100mg/ml；对所试厌氧菌(如脆弱拟杆菌，消化球菌，消化链球菌，痤疮丙酸杆菌和颗粒丙酸杆菌的MIC值在12.5～200mg/ml.)
(二)体内抗菌保护实验结果见表6。
1.不同用药部位、不同提取工艺的头花蓼样品口服给药，对小鼠金黄色葡萄球菌MSSA43感染具有一定的治疗作用。头花蓼减压干燥粉、头花蓼喷雾干燥粉、根提醇物、叶提醇物、茎提醇物、鲜品醇提物、鲜品水提物对金黄色葡萄球菌MSSA43感染小鼠的ED50分别为13.62、6.87、16.14、9.14、15.29、13.62、23.47g生药/kg。
2.不同用药部位、不同提取工艺的头花蓼样品口服给药，对大肠埃希菌994感染小鼠体内保护作用较差，当给药浓度为1.2g/ml生药浓度、0.8g/ml生药浓度、0.4g/ml生药浓度，小鼠存活率均大于或等于60％，与感染对照组比较均无显著性差异(P＞0.05)。
表5 不同药用部位、不同提取、制备工艺的头花蓼样品的体外抗菌谱
| 细菌(菌号) | (W-1-2)喷雾干燥(mg/ml) | (W-1-3)减压干燥(mg/ml) | (W-1-4)根醇提取物(mg/ml) | (W-1-5)茎醇提取物(mg/ml) | (W-1-6)叶醇提取物(mg/ml) | (W-1-7)种子提物(mg/ml) | (W-1-8)鲜品醇提(mg/ml) | (W-1-9)鲜品水提(mg/ml) | (W-1-10)药75％乙醇提物(mg/ml) | (W-1-12) | (W-1-14a)水煮醇沉溶物(mg/ml) | (W-1-14b)水提醇沉物(mg/ml) | 阳性对照没食子酸(mg/ml) | 阳性对照环丙沙星(μg/ml) | 阳性对照头孢三嗪钠(μg/ml) | 阳性对照洁尔阴(mg/ml) | 阳性对照氟康唑(μg/ml) |
| 痢疾杆菌铜绿假单胞菌994肺炎克雷伯菌9938肺炎克雷伯菌9939大肠埃希菌992大肠埃希菌993大肠埃希菌ATCC25922变形杆菌993变形杆菌994滕黄八叠球菌金黄色葡萄球菌209p金黄色葡萄球菌9981金黄色葡萄球菌9982金黄色葡萄球菌9983表葡球菌994表葡球菌995表葡球菌9916卡他氏球菌3C群链球菌A型溶血性链球菌淋球菌1淋球菌2淋球菌3淋球菌4淋球菌5淋球菌6淋球菌7淋球菌8淋球菌9淋球菌10淋球菌11淋球菌12淋球菌13 | 1001002525256.2525252512.56.2511.512.512.56.2512.56.254004004003.123.120.050.20.10.0250.0250.390.0250.0250.10.390.05 | 502550502512.550505012.56.256.25256.256.256.256.251001001000.780.780.01250.780.0250.780.780.780.780.780.050.780.05 | 100501001005050100100100502550505050505020020020025256.2550506.256.256.256.25506.25256.25 | 505050100251.565025250.390.390.780.390.390.78256.2540040040025250.10.20.2250.20.2250.20.22525 | 12.562.512.512.53.120.786.253.123.120.391.560.780.780.780.780.780.7812.512.512.51.561.560.0036.2512.56.250.030.036.256.256.250.0250.003 | 3.121.5612.512.50.390.056.256.256.250.050.050.050.050.050.050.390.3912.512.512.51.561.560.391.563.123.121.561.563.123.121.561.560.39 | 6.251001001000.390.396.253.126.250.390.050.050.050.050.393.120.392002002000.0250.0251.560.20.21.560.0250.10.780.21.561.560.025 | 2525252512.53.1225252512.51.561.561.561.563.12251.564004004003.12＞503.120.390.391.560.393.120.051.5612.56.250.39 | 2512.525500.780.112.56.256.250.10.10.10.10.10.780.781.562525256.256.251.566.253.123.126.250.11.561.563.126.253.12 | 2002004004001001002002002001002512.56.256.251001005040040040012.5253.121.561.5612.51.561.563.123.123.123.121.56 | 252550502512.512.5252512.51.5612.51.561.563.12256.254004004003.123.120.78＞100＞1001.563.120.780.2250.780.780.78 | 251004004003.123.1220050501.560.10.050.050.786.253.120.0520020020012.56.256.2512.56.256.256.256.256.256.2512.56.256.25 | 12.512.512.56.253.123.126.2512.512.512.512.512.56.256.2512.512.56.2512.512.512.51.560.780.050.780.050.780.050.050.050.20.780.780.01 | 44440.50.50.5161640.5440.581120.520.780.780.0150.780.780.390.01250.0150.0150.780.780.780.015 | ＞128＞128＞1286412840.03＞1282448888＞1284＞128＞128160.00156.250.00150.00150.00156.250.00150.01250.00156.256.250.390.0015 | NtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNt88862.531.51616844112 | NtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNtNt |
| 淋球菌14淋球菌15淋球菌16淋球菌17淋球菌18淋球菌19淋球菌20白色念珠菌011白色念珠菌012白色念珠菌013白色念珠菌014白色念珠菌015白色念珠菌016白色念珠菌017白色念珠菌018白色念珠菌019白色念珠菌0110白色念珠菌0111白色念珠菌0112白色念珠菌0113白色念珠菌0114白色念珠菌0115白色念珠菌0116白色念珠菌0117白色念珠菌0118白色念珠菌0119白色念珠菌0120 | 0.0250.0250.10.10.050.390.05400400400400400200200200400400400400400200400400400400400400 | 0.780.050.780.780.780.780.78200200200200200100100200200200200100200200100200200200200200 | 6.256.25506.256.256.2525400400400400400200200400400400400400400400400400400400400400 | 0.20.2252 50.20.20.39200200200200200400400100200200200200200200200200200200200200 | 0.396.256.250.0251.561.561.562 52 550502512.5256.2512.512.52512.512.525252512.512.52525 | 1.561.561.561.560.391.561.56252550252512.512.56.2512.512.5252512.512.512.512.52512.512.512.5 | 0.256.560.20.21.561.561.56200400200200200200400100200200200400200200400200200200200200 | 0.390.3912.53.123.120.396.25400400400400400200400200400400400400400400400400400400400400 | 1.560.20.780.781.250.781.565050501005025501002550251002525502550252550 | 3.126.253.126.251.561.563.12＞400＞400400400400＞400＞400＞400＞400400400＞400＞400＞400＞400＞400＞400＞400＞400＞400 | 0.20.20.780.780.20.20.78400400400400400200400200200400400400400400400400400400400400 | 6.256.2512.512.56.256.2512.5400400400400400200400200100200200400200400400200400400200400 | 0.010.011.560.390.390.780.7825252512.525255012.512.512.5252512.56.2512.525256.2512.525 | 0.10.01250.780.0150.20.0250.264128128＞128＞128128＞128128＞128＞12864＞128＞128＞128128＞1283264＞128＞128 | 0.01250.01256.250.00150.1250.050.39128＞128＞128＞128＞128＞128＞128＞128128＞128128＞128＞128＞128＞128＞128128128＞128＞128 | 12818431.2516831.254431.25862.581284462.5462.5816448 | NtNtNtNtNtNtNt0.030.06221240.030.50.50.250.1250.1250.584820.030.125 |
注：Nt＝not tested(没有试验)
表6 不同头花蓼提取物的体内保护实验结果
| 感染菌株(菌株号)(感染菌量CFU/ml) | 药物 | 编号 | ED50(g/kg)95％可信限 | P值 |
| 金黄色葡萄球菌MSSA43(2.5×105)大肠埃希菌994(3.0×105) | 喷雾干燥粉减压干燥粉根醇提物茎醇提物叶醇提物鲜品醇提鲜品水提w-1-2加辅料制成的颗粒氟哌酸胶囊喷雾干燥粉减压干燥粉根醇提物茎醇提物叶醇提物鲜品醇提鲜品水提w-1-2加辅料制成的颗粒氟哌酸胶囊 | w-1-2w-1-3w-1-4w-1-5w-1-6w-1-8w-1-9w-1-12阳性对照w-1-2w-1-3w-1-4w-1-5w-1-6w-1-8w-1-9w-1-12阳性对照 | 6.87(0-1000)13.62(0-1000)16.14(9.11-23.12)15.29(0-1000)9.14(0-1000)13.62(3.89-19.94)23.47(17.77-33.07)＞3025.96(16.09-35.24)(mg/kg)＞30＞30＞30＞30＞30＞30＞30＞3057.97(43.33-78.24)(mg/kg) | P＜0.05P＜0.05P＜0.05P＜0.05P＜0.05P＜0.05P＜0.05P＞0.05P＞0.05P＞0.05P＞0.05P＞0.05P＞0.05P＞0.05P＞0.05P＞0.05 |
试验结果说明：
1.不同药用部位的体外抗菌活性强度依次为：种子＞叶＞茎＞根。种子和叶的抗菌活性明显强于茎和根；而种子和叶之间、茎和根之间的抗菌活性并无明显差异。种子来源和采集都较困难，而根关系到药材的再生以及资源、环境保护，因此采用叶和茎或者地上部分做药材较合适。
2.全草、鲜品用95％乙醇提取的样品的体外抗菌活性明显强于用水提取的样品。
3.全草、干品水提后用减压干燥，还是用喷雾干燥，对样品的体外抗菌活性无明显影响。
4.头花蓼浸膏粉的体外抗菌活性明显强于样品(w-1-12)。
5.鲜品醇提物对金黄色葡萄球菌感染的体内疗效强于鲜品水提物。
6.头花蓼喷雾干燥粉对金黄色葡萄球菌感染的体内疗效强于头花蓼减压干燥粉强于热淋清颗粒。
7.叶95％乙醇提物对金黄色葡萄球菌感染的体内疗效强于根95％乙醇提物和茎95％乙醇提物。
8.不同用药部位、不同提取工艺的头花蓼样品口服给药，对大肠埃希菌994感染小鼠体内保护作用较差。
试验三：镇痛活性研究
实验方法：
就W-1-2进行了扭体法、热板法、热辐射法三种疼痛模型的研究。
实验结果：
1.对醋酸诱发的小鼠疼痛有一定的镇痛作用，量效关系明显，有效剂量为34.8g/kg。
2.对辐射热刺激造小鼠疼痛模型有一定镇痛作用。
实验结果说明：本发明提取物具有一定的镇痛作用。
试验四：利尿活性研究
实验方法：
就W-1-2进行了导尿管集尿法和代谢笼法两种利尿试验。
实验结果：17.4g/kg剂量对麻醉家兔有明显的利尿作用；8.7g/kg剂量对正常大鼠有明显的利尿作用。二试验均未显出量效关系。
试验结果说明：本发明提取物就有一定的利尿作用。
试验五：治疗肾盂肾炎的研究
实验方法：SD大鼠肾实质内接种大肠埃希氏菌ATCC-25922，制做大鼠肾盂肾炎模型。以口服给药方式探讨了头花蓼浸膏粉(w-1-2)对肾盂肾炎的疗效。
实验结果：头花蓼浸膏粉6.0g/kg(折合生药量为52.32g/kg)对肾盂肾炎有较为明显的疗效，与模型对照相比，给药(i.g.)后3、4、5、6、7天能显著减少尿液中的白细胞数量及隐血，但对尿液其它生化成份没有明显影响。
结果说明：本专利申请的样品对肾盂肾炎有一定的疗效。
试验六：排石活性研究
实验方法：用乙二醇饮水法造成大鼠草酸钙肾结石模型，造模同时预防给予头花蓼浸膏粉(w-1-2)13.1、26.2、52.4g原生药/kg三个剂量，连续7天。
实验结果：头花蓼浸膏粉26.2g原生药/kg剂量可显著性降低动物尿液中草酸、尿酸的含量，以及肾脏中草酸钙结晶的分布与数量。
结果说明：头花蓼浸膏粉对大鼠草酸钙肾结石模型具有明显的保护作用。
Claims (11)
1.一种头花蓼提取物，其特征在于由下列方法制备得到：
a.由头花蓼全草的鲜品或干品用水分两次煎煮或用醇水混合液分二至三次回流提取，每次1-2小时，合并煎煮液或提取液，过滤浓缩至20℃时的相对密度为1.2，喷雾干燥或减压干燥得到；或者
b.由头花蓼全草或其水提药渣经二氧化碳超临界萃取得到。
2.根据权利要求1的提取物，其中头花蓼选用其地上部分。
3.根据权利要求1的提取物，其中使用水作为提取溶媒。
4.根据权利要求1的提取物，其中的醇水混合物是75％乙醇水溶液或95％乙醇水溶液。
5.根据权利要求1-4之一的提取物，其特征在于头花蓼地上部分包括头花蓼茎、叶、花、和/或种子或者它们的混合物。
6.根据权利要求1-4之一的提取物，其特征在于头花蓼地上部分是叶、花和茎。
7.根据权利要求1-4之一的提取物，其特征在于头花蓼地上部分是叶、种子和茎。
8.根据权利要求1-4之一的提取物，其特征在于头花蓼地上部分是叶和茎。
9.一种药物组合物，其含有权利要求1-8之一的提取物和可药用辅料。
10.根据权利要求9的组合物，其是片剂。
11.根据权利要求9或10的药物组合物在抗菌、抗炎、镇痛、利尿、或治疗肾盂肾炎和排石方面的用途。
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| CN100535655C (zh) * | 2006-06-22 | 2009-09-02 | 成都中医药大学 | 头花蓼药材的检测方法 |
| CN101664446A (zh) * | 2009-09-28 | 2010-03-10 | 贵州威门药业股份有限公司 | 热淋清浸膏及其制备方法和用途 |
| CN102526218B (zh) * | 2012-01-05 | 2013-07-31 | 贵州威门药业股份有限公司 | 制备头花蓼提取物的方法和头花蓼提取物 |
| CN102526219B (zh) * | 2012-01-05 | 2013-07-31 | 贵州威门药业股份有限公司 | 热淋清颗粒提取物及其制备方法和用途 |
| CN104224943A (zh) * | 2013-06-21 | 2014-12-24 | 北大方正集团有限公司 | 用于治疗慢性前列腺炎的中药组合物、制备方法和用途 |
| CN103550310B (zh) * | 2013-10-30 | 2015-08-19 | 浙江百草中药饮片有限公司 | 一种头花蓼降糖提取物口服液的制备方法 |
| CN103536663B (zh) * | 2013-10-30 | 2015-08-19 | 浙江百草中药饮片有限公司 | 一种头花蓼降糖提取物片剂的制备方法 |
| CN103550311B (zh) * | 2013-10-30 | 2015-08-19 | 浙江百草中药饮片有限公司 | 一种头花蓼提取物及其制备方法和应用 |
| CN105434555A (zh) * | 2015-12-30 | 2016-03-30 | 贵州弘康药业有限公司 | 一种热淋清制剂的制作方法 |
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2003
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