CN102119946A - 一种三七有效组分及其制备方法与用途 - Google Patents
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Abstract
本发明提供一种三七有效组分,将药材通过加热提取,浓缩,反相硅胶柱分离,洗脱,洗脱液浓缩干燥,再用制备液相色谱继续分离,收集溶液,溶液经浓缩干燥后得到有效组分。本发明提供的三七有效组分可在制备治疗、预防心血管疾病药物中的应用。本发明方法设计合理,能快速准确地得到有效成分,在生产中更易于药物的质量控制。
Description
技术领域
本发明属于中医领域,涉及一种从三七中提取有效组分及其制备方法与用途,该有效组分通过提取,反相柱中压分离,制备液相分离而获得,可用于制备治疗心血管疾病的药物。
背景技术
心血管疾病是危害人类健康的第一杀手,近年来,随着我国人口老年化以及人们工作、生活、饮食结构及环境等的变化,冠心病等心脑血管疾病的发生率也逐年增多,严重威胁着人民的身心健康。天然产物中许多活性物质具有抗心肌缺血、缺氧作用,其中一些已开发成治疗冠心病和心绞痛的新药。因而从天然产物中寻找具有抗心肌缺血、缺氧生理活性的有效物质,是发现、开发新药的有效途径之一。我国药用生物资源十分丰富,其生理活性物质是研究和发现新药先导化学物,开发新药的天然宝库。目前,我国从天然产物中提取活性物质,用于开发成治疗冠心病、安全性好、毒性低的新药还很少,从天然产物中提取活性物质,开发成具有抗心肌缺血,用于治疗冠心病和心绞痛的新药,具有重要应用价值和广阔发展前景。
三七为五加科植物三七Panax notoginseng (Burk.) F. H. Chen的干燥根。中医认为,其味甘、微苦,性温,归肝、胃经。具有散瘀止血,消肿定痛之功效,适用于治疗咯血,吐血,衄血,便血,崩漏,外伤出血,胸腹剌痛,跌扑肿痛等。现代研究表明,三七中主要含人参皂甙(Ginsenosides)Rb1、 Rd、Re、Rg1、Rg2、Rh,20-O-葡萄糖人参皂甙Rf ,三七皂甙(Notoginsenoside)R1、R2、R3、 R4,七叶胆皂甙(Gypeno-side)ⅩⅦ,尚含人参皂甙Rb2。还含挥发油,有 -及-愈创烯(-,-guaiene),另外有-古巴烯(-copaene)、-愈创烯、花柏烯(cuparene)、-,-, γ-榄香烯(-,-,-elemene)、-依兰油烯(-muurolene)、-古芸烯(- gurjunene)、十六酸甲酯、十六酸乙酯、十七碳二烯酸甲酯、十八碳二烯酸乙酯、邻苯二甲酸二叔丁酯(benzene-diformic acid ditert-butylate)、十八碳二烯酸、异丙苯、环十二碳酮(cy-clodode-canone)、1-甲基-4-过氧甲硫基[2,2,2]辛烷、十四烷、十六烷、十七烷、十八烷、十九烷、廿烷、廿一烷、廿二烷。水提取液中含一种具止血活性的三七素(N-oxalo-L- ,-diaminopro-pionic acid)。另含槲皮素、三七黄酮B、-谷甾醇、-谷甾醇-D-葡萄糖甙、蔗糖
发明内容
本发明的目的在于提供一种三七有效组分,通过以下步骤制备获得:将三七药材粉碎后加入乙酸乙酯和乙醇,加热提取,药渣加乙醇水溶液提取,将提取液浓缩成浸膏,用反相硅胶柱对其进行分离,首先用低浓度甲醇作为流动相,得洗脱液I,弃之,然后改用高浓度甲醇作为流动相,得洗脱液II,将洗脱液II浓缩干燥后得样品;用制备液相色谱继续分离得到的样品;制备色谱的分离条件:色谱柱为制备柱,流动相为水和乙腈,梯度洗脱。
具体制备步骤如下:取三七药材,将其粉碎后加入体积比为1:1的乙酸乙酯和乙醇,加热回流1小时,提取2次,滤液合并得提取液I。药渣加入70%乙醇,加热回流1小时,提取2次,滤液合并得提取液II,将提取液II浓缩成浸膏,用50%甲醇溶液溶解浸膏,采用ODS-C18柱对其进行分离,首先用5%甲醇溶液作为流动相,得洗脱液I,然后改用60%甲醇溶液作为流动相,得洗脱液II,将洗脱液II浓缩干燥后得样品;用制备液相色谱继续分离得到的样品:制备色谱的分离条件:色谱柱为Agilent制备柱(Zorbax SB-C18;21.2mm250mm),流动相为水A和乙腈B,梯度洗脱程序如下:0min时,流动相A 为90%的水,流动相B为10%的乙腈溶液;15min时,流动相A 为72%的水,流动相B为28%的乙腈溶液;流速为10ml/min,柱温为室温;样品经制备液相色谱分离,在3.0~7.4min时间段收集溶液,溶液经浓缩干燥后得到有效组分。
本发明的另一个目的是提供所述三七有效组分在制备治疗心血管疾病的药物中的应用。经药理实验证明,本发明提供的三七有效组分对心肌细胞有保护作用。
本发明提供的三七有效组分作为活性成分,加入药剂学上接受的辅料,按照药剂学上记载的制剂的制备方法制成制剂。
药物的制剂形式为液体制剂或固体制剂,包括注射液、滴注液、粉针剂、颗粒剂、片剂、冲剂、散剂、口服液、糖衣片剂、薄膜衣片剂、肠溶衣片剂、胶囊剂、硬胶囊剂、软胶囊剂、口含剂、颗粒剂、丸剂、膏剂、丹剂、喷雾剂、滴丸剂 、崩解剂、口崩片、微丸等。
本发明提供的三七有效组分可在制备治疗、预防心血管疾病药物中的应用。本发明提供的制备方法设计合理,能快速准确地得到有效成分,在生产中更易于药物的质量控制。
具体实施方式
下面将结合实施例进一步详细说明本发明的实质内容和有益效果,该实施例仅用于说明本发明而非对本发明的限制。
实施例一 三七有效组分的制备
将三七药材粉碎后加入乙酸乙酯和乙醇,加热提取,药渣加乙醇水溶液提取,将提取液浓缩成浸膏,用反相硅胶柱对其进行分离,首先用低浓度甲醇作为流动相,得洗脱液I,弃之,然后改用高浓度甲醇作为流动相,得洗脱液II,将洗脱液II浓缩干燥后得样品;用制备液相色谱继续分离得到的样品;制备色谱的分离条件:色谱柱为制备柱,流动相为水和乙腈,梯度洗脱。
实施例二 三七有效组分的制备
取三七药材,将其粉碎后加入体积比为1:1的乙酸乙酯和乙醇,加热回流1小时,提取2次,滤液合并得提取液I。药渣加入70%乙醇溶液,加热回流1小时,提取2次,滤液合并得提取液II,将提取液II浓缩成浸膏,用50%甲醇溶液溶解浸膏,采用ODS-C18柱对其进行分离,首先用5%甲醇溶液作为流动相,得洗脱液I,然后改用60%甲醇溶液作为流动相,得洗脱液II,将洗脱液II浓缩干燥后得样品;用制备液相色谱继续分离得到的样品:制备色谱的分离条件:色谱柱为Agilent制备柱(Zorbax SB-C18;21.2mm250mm),流动相为水A和乙腈B,梯度洗脱程序如下:0min时,流动相A 为90%的水,流动相B为10%的乙腈溶液;15min时,流动相A 为72%的水,流动相B为28%的乙腈溶液;流速为10ml/min,柱温为室温;样品经制备液相色谱分离,在3.0~7.4min时间段收集溶液,溶液经浓缩干燥后得到有效组分。
实施例三 滴丸制剂的制备
取三七有效组分0.5g与10.5g聚乙二醇-20000混合均匀,加热熔融,化料后移至滴丸滴灌中,药液滴至6~8℃液体石蜡中,除油,制得滴丸400粒。
实施例四 冻干粉针剂的制备
取三七有效组分0.5g、葡萄糖4.5g、硫代硫酸钠0.9g和蒸馏水1000ml,上述组分混合均匀后,分装400支,冷冻干燥,即得。
实施例五 三七组分的活性评价实验
1.三七组分对H2O2损伤心肌细胞的保护作用
体外培养H9C2心肌细胞,培养液为DMEM(高糖)+10%FBS(G)+1%非必需氨基酸+0.1%双抗。取对数生长期细胞置于96孔细胞培养板上,恒温培养24 h后,加入200μmol/mL H2O2损伤心肌细胞30 min,再加入终浓度为50μg/mL的三七组分孵育24 h,采用MTT法测定细胞活力。结果表明,该组分对H2O2损伤心肌细胞的保护率为16.61%。
2. 三七组分对缺氧复氧损伤心肌细胞的保护作用
体外培养H9C2心肌细胞,培养液为DMEM(高糖)+10%FBS(G)+1%非必需氨基酸+0.1%双抗。取对数生长期细胞置于96孔细胞培养板上,恒温培养24 h后,在缺氧小室中培养6 h。缺氧结束后,取出细胞培养板加入经无糖Hank’s稀释的终浓度为50μg/mL的三七组分,在正常培养条件下孵育6h小时,取细胞培养上清液测定乳酸脱氢酶(LDH)含量。结果表明,该组分对缺氧复氧损伤的心肌细胞保护率为6.52%。
Claims (5)
1.一种三七有效组分,其特征在于,通过以下步骤获得:取三七药材,将其粉碎后加入体积比为1:1的乙酸乙酯和乙醇,加热回流1小时,提取2次,滤液合并得提取液I;药渣加入70%乙醇溶液,加热回流1小时,提取2次,滤液合并得提取液II,将提取液II浓缩成浸膏,用50%甲醇溶液溶解浸膏,采用ODS-C18柱对其进行分离,首先用5%甲醇溶液作为流动相,得洗脱液I,然后改换60%甲醇溶液作为流动相,得洗脱液II,浓缩干燥后得样品,用制备液相色谱继续分离得到的样品,梯度洗脱,收集溶液,溶液经浓缩干燥后得到有效组分。
2.根据权利要求1所述的一种三七有效组分,其特征在于,制备色谱的分离条件:色谱柱为Agilent制备柱,Zorbax SB-C18; 21.2mm′250mm,流动相为水A和乙腈B,梯度洗脱程序为:0min,10%B;15min,28%B;流速为10ml/min,柱温为室温;样品经制备液相色谱分离,在3.0~7.4min时间段收集溶液,溶液经浓缩干燥后得到有效组分。
3.根据权利要求1所述的一种三七有效组分在制备治疗心血管疾病的药物中的应用。
4.根据权利要求3所述的应用,其特征在于,所述药物由三七有效组分加入药剂学上可接受的辅料,按照药剂学上记载的制剂制备方法制成。
5.根据权利要求4所述的应用,其特征在于,所述药物的制剂形式为液体制剂或固体制剂。
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