CN103923074B - 一种从葫芦巴中提取牡荆素、葫芦巴碱的方法 - Google Patents

一种从葫芦巴中提取牡荆素、葫芦巴碱的方法 Download PDF

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CN103923074B
CN103923074B CN201410156823.3A CN201410156823A CN103923074B CN 103923074 B CN103923074 B CN 103923074B CN 201410156823 A CN201410156823 A CN 201410156823A CN 103923074 B CN103923074 B CN 103923074B
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vitexin
trigonella
trigonelline
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CN103923074A (zh
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刘海峰
姚晨
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SHENGSHI HESHENG BIOLOGICAL TECHNOLOGY Co Ltd
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    • C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
    • C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
    • C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
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    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D213/79—Acids; Esters
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract

本发明公开了一种从葫芦巴中同时提取牡荆素、葫芦巴碱的方法，通过以下步骤制备完成：从一定量的葫芦巴种子和葫芦巴叶获取得率为20％～35％的含有葫芦巴碱和牡荆素的水提物；向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.1～0.5，水解1-2小时，待充分析出结晶A后，再采用浓度为50％-90％的乙醇溶液进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出结晶A后的溶液进行喷雾干燥获得产品葫芦巴碱。该方法先将葫芦巴中的中药有效成分充分的溶解在水溶液中后，再进行牡荆素和葫芦巴碱的提取，大大地提高了牡荆素和葫芦巴碱的提取率和提取纯度。

Description

一种从葫芦巴中提取牡荆素、葫芦巴碱的方法
技术领域
本发明涉及中药中提取有效成分的方法，具体涉及从葫芦巴中同时提取牡荆素、葫芦巴碱的方法。
背景技术
草本植物葫芦巴含有的化学成分有葫芦巴碱(trigonellinelline)，薯蓣皂甙元葡萄糖甙(diosgenin-B-D-blucoside)、牡荆素(vitexin)、牡荆素-7-葡萄糖甙、异牡荆素(saponaretin)、异荭草素(isoorientin)(vitexin-7-glucoside)、葫芦巴甙Ⅰ、∏(viceninⅠ,∏)
其中，牡荆素主要功能是活血化瘀，理气通脉；用于瘀血阻脉所致的胸痹，症见胸闷憋气，心前区刺痛、心悸健忘、眩晕耳鸣。目前牡荆素主要用于治疗心血管疾病，不过用于治疗心血管疾病对牡荆素纯度要求非常的高，一般要求>98％(HPLC)。
目前，常采用从草本植株中提取的牡荆素和葫芦巴碱的工艺相对复杂，且成分复杂，纯度很难达到98％(HPLC)，使得提取的牡荆素药效难以达到预期的效果。
发明内容
针对现有技术中的上述不足，本发明提供的从葫芦巴中同时提取牡荆素、葫芦巴碱的方法，其先将葫芦巴中的中药有效成分充分的溶解在水溶液中后，再进行牡荆素和葫芦巴碱的萃取，大大地提高了牡荆素和葫芦巴碱的提取率和提取纯度。
为了达到上述发明目的，本发明的目的是采用下述技术方案来实现的：
1)获取含有葫芦巴碱和牡荆素的水提物
将葫芦巴种子和葫芦巴叶进行洗净；
将葫芦巴种子在25MPa、90～120℃的条件下放置1h～3h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；
向上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的6-9倍的纯净水，浸泡0.5h～1h，煮沸10-20分钟，获取过滤液A；
向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡0.5h～1h，煮沸10-20分钟，获取过滤液B；
将上述过滤液A和过滤液B混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物；
2)获取牡荆素
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.1～0.5，水解1-2小时，待充分析出晶体A后，再采用浓度为50％-90％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
本发明的有益效果为：将葫芦巴种子和葫芦巴叶粉碎后，将其含有的中药有效成分充分的溶解在水溶液中，再采用一定浓度的盐酸和乙醇溶液进行萃取，简化了提取工艺，且有效地提高了牡荆素和葫芦巴碱的萃取率；将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99％(HPLC)以上。
具体实施方式
下面结合具体实施例对本发明从葫芦巴中同时提取牡荆素、葫芦巴碱的方法作进一步地说明，但下述实施例不以任何方式限制本发明。
实施例1
取一定量的葫芦巴种子和葫芦巴叶进行洗净；将葫芦巴种子在25MPa、90℃的条件下放置1h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；将上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的6倍的纯净水，浸泡0.5h，煮沸10分钟，获取过滤液；向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡0.5h，煮沸10分钟，获取过滤液；将上述两次过滤液混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物。
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.1，水解1小时，待充分析出晶体A后，再采用浓度为50％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
采用本实施例的方法获取的含有葫芦巴碱和牡荆素的水提物的得率为21％，并将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99.5％(HPLC)。
实施例2
取一定量的葫芦巴种子和葫芦巴叶进行洗净；将葫芦巴种子在25MPa、100℃的条件下放置1h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；将上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的7倍的纯净水，浸泡0.6h，煮沸15分钟，获取过滤液；向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡0.7h，煮沸10分钟，获取过滤液；将上述两次过滤液混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物。
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.3，水解2小时，待充分析出晶体A后，再采用浓度为75％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
采用本实施例的方法获取的含有葫芦巴碱和牡荆素的水提物的得率为25％，并将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99.2％(HPLC)。
实施例3
取一定量的将葫芦巴种子和葫芦巴叶进行洗净；将葫芦巴种子在25MPa、110℃的条件下放置2h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；将上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的8倍的纯净水，浸泡1h，煮沸15分钟，获取过滤液；向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡0.8h，煮沸20分钟，获取过滤液；将上述两次过滤液混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物。
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.35，水解2小时，待充分析出晶体A后，再采用浓度为75％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
采用本实施例的方法获取的含有葫芦巴碱和牡荆素的水提物的得率为27％，并将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99.4％(HPLC)。
实施例4
取一定量的将葫芦巴种子和葫芦巴叶进行洗净；将葫芦巴种子在25MPa、90～120℃的条件下放置3h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；将上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的9倍的纯净水，浸泡1h，煮沸20分钟，获取过滤液；向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡1h，煮沸20分钟，获取过滤液；将上述两次过滤液混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物。
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.5，水解2小时，待充分析出晶体A后，再采用浓度为90％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
采用本实施例的方法获取的含有葫芦巴碱和牡荆素的水提物的得率为30％，并将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99.1％(HPLC)。
实施例5
将葫芦巴种子和葫芦巴叶进行洗净；取一定量葫芦巴种子在25MPa、115℃的条件下放置2.5h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；将上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的7倍的纯净水，浸泡1h，煮沸20分钟，获取过滤液；向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡1h，煮沸20分钟，获取过滤液；将上述两次过滤液混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物。
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.4，水解1-2小时，待充分析出晶体A后，再采用浓度为75％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
采用本实施例的方法获取的含有葫芦巴碱和牡荆素的水提物的得率为34％，并将获取的牡荆素和葫芦巴碱采用高效液相色谱法定量分析，测得采用本方法获取的牡荆素纯度达到99.6％(HPLC)。

Claims (3)

1.一种从葫芦巴中同时提取牡荆素、葫芦巴碱的方法，其特征在于，通过以下步骤制备完成：
1)获取含有葫芦巴碱和牡荆素的水提物
将葫芦巴种子和葫芦巴叶进行洗净；
将葫芦巴种子在25MPa、90～120℃的条件下放置1h～3h，使其充分膨化后进行粉碎，获得葫芦巴种子粉碎物；将葫芦巴叶粉碎成粉末，并过40目筛网，获取葫芦巴叶粉碎物；
向上述获取的葫芦巴种子粉碎物和葫芦巴叶粉碎物中加入两者总重量的6-9倍的纯净水，浸泡0.5h～1h，煮沸10-20分钟，获取过滤液A；
向获取过滤液A之后得到的滤渣中加入滤渣重量7倍的纯净水，浸泡0.5h～1h，煮沸10-20分钟，获取过滤液B；
将上述过滤液A和过滤液B混合，搅拌均匀，浓缩成膏状物，获得含有葫芦巴碱和牡荆素的水提物；
2)获取牡荆素
向上述获取的含有葫芦巴碱和牡荆素的水提物中加入盐酸，并将溶液的pH调整至pH＝0.1～0.5，水解1-2小时，待充分析出晶体A后，再采用浓度为50％-90％的乙醇溶液对晶体A进行重结晶得到晶体a；将上述晶体a溶解后加入95％的乙醇溶液析出牡荆素晶体，并对析出晶体A后过滤得到的溶液进行喷雾干燥获得产品葫芦巴碱。
2.根据权利要求1所述的从葫芦巴中同时提取牡荆素、葫芦巴碱的方法，其特征在于：步骤2)中对晶体A进行重结晶时采用的乙醇溶液的浓度为75％。
3.根据权利要求1所述的从葫芦巴中同时提取牡荆素、葫芦巴碱的方法，其特征在于：步骤1)中含有葫芦巴碱和牡荆素的水提物的得率为20％～35％。
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