CN110025677B - 一种大黄提取物的制备方法 - Google Patents
一种大黄提取物的制备方法 Download PDFInfo
- Publication number
- CN110025677B CN110025677B CN201910474505.4A CN201910474505A CN110025677B CN 110025677 B CN110025677 B CN 110025677B CN 201910474505 A CN201910474505 A CN 201910474505A CN 110025677 B CN110025677 B CN 110025677B
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- Prior art keywords
- ethanol
- rhubarb
- ethyl acetate
- extract
- water
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Classifications
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
- A61K36/708—Rheum (rhubarb)
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- A—HUMAN NECESSITIES
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- A61K2236/30—Extraction of the material
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- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
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- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
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Abstract
本发明公开了一种大黄提取物的制备方法，步骤如下：将熟大黄药材粉碎成最粗粉，用水加热回流提取2‑4次，每次1‑2h，每次6‑10倍量水，首次多加2倍量，滤过，合并滤液，浓缩至密度1.10‑1.15g/ml(60℃)，放冷，加入2‑6倍体积量的乙醇，醇沉12‑36小时，醇沉物备用，醇沉上清液减压回收乙醇至无醇味(密度为1.10‑1.15g/ml(60℃))，用1‑3倍体积量的乙酸乙酯萃取2‑6次，合并乙酸乙酯层萃取液，回收乙酸乙酯后得没食子酸部位，与醇沉物混合均匀，减压(60℃)干燥，粉碎，得大黄提取物，该方法可有效提取出大黄中具有保肝利胆的有效成分，作为大黄的有效部位应用于药品制备。
Description
技术领域
本发明属于医药技术领域，具体涉及一种大黄提取物的制备方法。
背景技术
大黄(Rhubarb)为历代医家本草和历版《中国药典》收载的常用中药，是传统泻下类中药的代表，来源于蓼科植物掌叶大黄Rheum palmatum L.、唐古特大黄RheumtanguticumMaxim.exBalf.或药用大黄Rheum officinaleBaill.的干燥根及根茎。大黄具多类药效活性成分，其中以蒽醌类、二蒽酮类、茋类、鞣质和多糖类成分，主要有调节胃肠功能、抗病原微生物、抗肿瘤、保护心脑血管、抗炎、保肝及抗衰老等多种药理活性作用。
鞣质类：20世纪80年代以来，随着大黄泻下以外新功效的深入研究，特别是大黄鞣质降低血清尿素氮活性的发现，使得大黄鞣质的化学成分研究不断深入。鞣酸等是良好的自由基活性氧的清除剂，国外对大黄的化学成分进行研究表明，经各种层析柱从大黄水提物中得到一淡褐色粉末，相对分子质量约2800的缩合型鞣质。
多糖类：多糖类是大黄的另外一类重要组分，从大黄根及根茎中得到DHP-I和DHP-2两种酸性多糖，平均相对分子质量分别为11000和25000。TLC和GC分析表明2种多糖的糖组成完全相同，主要由葡萄糖、半乳糖、阿拉伯糖、鼠李糖、来苏糖、木糖、葡萄糖醛酸、半乳糖醛酸组成。
蒽醌、蒽酮类：是大黄中的一类主要活性成分，具有泻下、抗菌活性。
二苯乙烯类：是大黄的一类重要成分，具有显著的抗清除自由基、抗衰老的作用。现代药理学研究表明，大黄药理作用主要有调节胃肠功能、抗病原微生物、抗肿瘤、保护心脑血管、抗炎、保肝及抗衰老等作用。
目前大黄提取过程中存在的问题是蒽醌含量偏高，导致副作用增加；而没食子酸含量偏低，保肝利胆的效果不明显。
发明内容
发明目的：本发明提供了一种大黄提取物的制备方法。
技术方案：一种大黄提取物的制备方法，包括以下步骤：
①将熟大黄药材粉碎成粗粉，用水加热回流提取，滤过，合并滤液；
②将合并的滤液减压浓缩，得水提浓缩液，放冷；
③加入乙醇，醇沉，醇沉物备用；
④醇沉上清液减压回收乙醇至无醇味，得醇提浓缩液；
⑤醇提浓缩液用乙酸乙酯萃取，合并乙酸乙酯层萃取液，回收乙酸乙酯后，与醇沉物混合均匀，减压干燥，粉碎，得大黄提取物。
所述的大黄提取物的制备方法，所述的步骤①，大黄原料与水之比为1︰6-1︰10；提取次数为2-3次；提取时间1-2小时。
所述的大黄提取物的制备方法，所述的步骤②，水提浓缩液的密度为1.10-1.15g/ml(60℃)。
所述的大黄提取物的制备方法，所述的步骤③，乙醇加入量为浓缩液体积的2-4倍量，醇沉时间为12-24小时。
所述的大黄提取物的制备方法，所述的步骤④，醇提浓缩液的密度为1.10-1.15g/ml(60℃)。
所述的大黄提取物的制备方法，所述的步骤⑤，乙酸乙酯每次用量为醇提浓缩液体积的1-3倍，萃取次数为2-6次。
有益效果：由于大黄蒽醌类存在一定的肝肾毒性，本发明的提取工艺在保证药效的前提下，大黄现工艺蒽醌含量较原工艺显著降低；没食子酸得到纯化，含量略有提升。
具体实施方式
以下通过实施例形式对本发明的上述内容再作进一步的详细说明，但不应将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容所实现的技术均属于本发明的范围。
实施例1：一种大黄提取物的制备方法，包括如下步骤：将熟大黄药材1kg粉碎成粗粉，用水加热回流提取2次，每次1h，第一次8倍量水，第二次6倍量水，滤过，合并滤液，浓缩至密度1.10g/ml(60℃)，放冷，加入2倍体积量的乙醇，醇沉12小时。醇沉物备用，醇沉上清液减压回收乙醇至无醇味(密度为1.10g/ml(60℃))，用等倍体积量的乙酸乙酯萃取4次，合并乙酸乙酯层萃取液，回收乙酸乙酯后得没食子酸部位，与醇沉物混合均匀，减压(60℃)干燥，粉碎，得大黄提取物。
实施例2：一种大黄提取物的制备方法，包括如下步骤：将熟大黄药材1kg粉碎成粗粉，用水加热回流提取3次，每次1.5h，第一次10倍量水，第二、三次8倍量水，滤过，合并滤液，浓缩至密度1.12g/ml(60℃)，放冷，加入4倍体积量的乙醇，醇沉18小时。醇沉物备用，醇沉上清液减压回收乙醇至无醇味(密度为1.12g/ml(60℃))，用2倍体积量的乙酸乙酯萃取3次，合并乙酸乙酯层萃取液，回收乙酸乙酯后得没食子酸部位，与醇沉物混合均匀，减压(60℃)干燥，粉碎，得大黄提取物。
实施例3：一种大黄提取物的制备方法，包括如下步骤：将熟大黄药材1kg粉碎成粗粉，用水加热回流提取3次，每次2h，第一次12倍量水，第二、三次10倍量水，滤过，合并滤液，浓缩至密度1.15g/ml(60℃)，放冷，加入3倍体积量的乙醇，醇沉24小时。醇沉物备用，醇沉上清液减压回收乙醇至无醇味(密度为1.15g/ml(60℃))，用3倍体积量的乙酸乙酯萃取2次，合并乙酸乙酯层萃取液，回收乙酸乙酯后得没食子酸部位，与醇沉物混合均匀，减压(60℃)干燥，粉碎，得大黄提取物。
实施例4：一种大黄提取物的制备方法，包括如下步骤：将熟大黄药材1kg粉碎成最粗粉，用水加热回流提取3次，每次1.5h，第一次10倍量水，第二、三次8倍量水，滤过，合并滤液，浓缩至密度1.12g/ml(60℃)，放冷，加入4倍体积量的乙醇，醇沉24小时。醇沉物备用，醇沉上清液减压回收乙醇至无醇味(密度为1.15g/ml(60℃))，用1倍体积量的乙酸乙酯萃取4次，合并乙酸乙酯层萃取液，回收乙酸乙酯后得没食子酸部位，与醇沉物混合均匀，减压(60℃)干燥，粉碎，得大黄提取物。
对比实施例1：参照华东理工大学、上海中医药大学申请的发明专利(申请号：201010501560；发明名称：一种中药组合物及其应用)，制备大黄提取物。
方法：准确称取酒制大黄饮片600g，加入6L体积百分比30％的乙醇水溶液进行回流提取，提取时间为60min，收集提取液；然后再向残渣中加入4.2L去离子水进行回流提取，提取时间为30min，收集提取液。将两次的提取液混合，冷却至室温，过滤，取滤液减压浓缩至体积/生药比约为2︰1，加入质量百分数为95％乙醇至含醇量达70％，于2～10℃静置过夜，过滤。将上述滤液于60℃以下减压浓缩至稠浸膏，然后于真空烘箱内60℃真空干燥至恒重，得制大黄鞣质提取物粉末约101g(大黄提取物II)以可见分光光度法测得其中大黄鞣质的含量为10％。以HPLC法测得其中没食子酸的含量为2％。色谱条件：以十八烷基硅烷键合硅胶为填充剂；体积分数为0.1％的乙酸为流动相A，以甲醇为流动相B，A︰B＝98︰2，流速1.0ml/min；检测波长270nm；柱温30℃)。将上述滤渣用质量百分数60％乙醇洗涤，然后于真空烘箱内60℃真空干燥至恒重，得到制大黄多糖提取物95g(大黄提取物I)(以可见分光光度法-苯酚硫酸法测得其中大黄多糖的含量为62％)。
实施例5：两种工艺提取物大黄蒽醌含量测定，测定方法参见2015版《中国药典》大黄项下含量测定方法，提取物中没食子酸含量如下髙效液相色谱法检测。
5.1总蒽醌照髙效液相色谱法(通则0512)测定。
色谱条件与系统适用性试验：以十八烷基硅烷键合硅胶为填充剂；以甲醇-0.1％磷酸溶液(85：15)为流动相；检测波长为254nm。
对照品溶液的制备精密称取芦荟大黄素对照品、大黄酸对照品、大黄素对照品、大黄酚对照品、大黄素甲醚对照品适量，加甲醇分别制成每lm l含芦荟大黄素、大黄酸、大黄素、大黄酚各80μg，大黄素甲醚40μg的溶液；分别精密量取上述对照品溶液各2ml，混匀，即得(每lml中含芦荟大黄素、大黄酸、大黄素、大黄酚各16μg，含大黄素甲醚8μg)。
供试品溶液的制备取本品粉末(过四号筛)约0.15g，精密称定，置具塞锥形瓶中，精密加入甲醇25ml，称定重量，加热回流1小时，放冷，再称定重量，用甲醇补足减失的重量，摇匀，滤过。精密量取续滤液5ml，置烧瓶中，挥去溶剂，加8％盐酸溶液10m l，超声处理2分钟，再加三氯甲烷10ml，加热回流1小时，放冷，置分液漏斗中，用少量三氯甲烷洗涤容器，并入分液漏斗中，分取三氯甲烷层，酸液再用三氯甲烷提取3次，每次10ml，合并三氯甲烷液，减压回收溶剂至干，残渣加甲醇使溶解，转移至10ml量瓶中，加甲醇至刻度，摇匀，滤过，取续滤液，即得。
测定法分别精密吸取对照品溶液与供试品溶液各10μl，注人液相色谱仪，测定，即得。
5.2游离蒽醌照高效液相色谱法(通则0512)测定。
色谱条件与系统适用性试验同〔含量测定〕总蒽醌项下。
对照品溶液的制备取〔含量测定〕总蒽醌项下的对照品溶液，即得。
供试品溶液的制备取本品粉末(过四号筛)约0.5g(大黄提取物粉末取约0.2g)，精密称定，置具塞锥形瓶中，精密加入甲醇25ml，称定重量，加热回流1小时，放冷，再称定重量，用甲醇补足减失的重量，摇匀，滤过，取续滤液，即得。
测定法分别精密吸取对照品溶液与供试品溶液各10μl，注入液相色谱仪，测定，即得。
5.3没食子酸含量测定照髙效液相色谱法(通则0512)测定。
色谱条件与系统适用性试验以十八烷基硅烷键合硅胶为填充剂，以甲醇-0.1％磷酸水溶液(5：95)为流动相，检测波长为273nm。
对照品溶液的制备取没食子酸对照品约13mg，精密称定，置100ml容量瓶中，50％甲醇溶液溶解，稀释并定容至刻度线，摇匀，精密移取10ml置25ml容量瓶中，50％甲醇溶液稀释，定容，摇匀，作为对照品溶液。
供试品溶液的制备取大黄提取物粉末(过四号筛)约0.25g，精密称定，平行称取2份，置具塞锥形瓶中，精密加入50％甲醇溶液50ml，称重，超声处理(功率250W，频率40kHz)30min，取出，放冷，50％甲醇溶液补重，过滤，取续滤液作为供试品溶液。
测定法分别精密吸取对照品溶液与供试品溶液各10μl，注入液相色谱仪，测定，即得。
5.4实验结果
5.4.1提取物提取得率
表1大黄提取物
5.4.2.大黄蒽醌含量
表2游离蒽醌含量比较
表3总蒽醌含量比较
5.4.3没食子酸含量
表4没食子酸含量比较
5.5结论
由表2、3可以看出，对比实施例1游离蒽醌总量为实施例4的8倍，实施例4游离蒽醌含量明显将低。对比实施例1总蒽醌总量为实施例4的6.6倍，实施例4总蒽醌含量明显将低。对比实施例1大黄蒽醌提取率较高，而实施例4条件下转移率明显降低；对比实施例1游离蒽醌/总蒽醌占比，较熟大黄饮片明显增加，而实施例4游离蒽醌/总蒽醌占比略有升高，变化意义不大。
由表4可以看出，现工艺没食子酸含量较现工艺略有升高，说明两种工艺均能提取没食子酸，但现工艺经过纯化，使得杂质含量较少，没食子酸提取率得到提升。
综上所述，由于大黄蒽醌类存在一定的肝肾毒性，在保证药效的前提下，大黄现工艺蒽醌含量较原工艺显著降低；没食子酸得到纯化，含量略有提升。
为进一步研究本发明工艺中关键步骤对大黄蒽醌类成分和没食子酸提取转移率影响，开展了分步测定研究。实验结果如下表5、6。
表5游离蒽醌含量对比
表6总蒽醌含量对比
由表5及表6可以看出，经过水提后，总蒽醌含量约为熟大黄饮片的1/3，游离蒽醌含量约为熟大黄饮片的1/5，表明采用水提的方式可以明显降低大黄蒽醌含量的提取率，且主要降低的为游离蒽醌的含量。提取液经过浓缩醇沉后，水提液大黄蒽醌含量大部分存留于上清液中，少部分存留在多糖沉淀中，并在浓缩醇沉滤过过程中略有损失。
由表5及表6可以看出，上清液经过乙酸乙酯萃取后，大黄蒽醌含量得到进一步降低，说明按本发明方法进行纯化没食子酸可以进一步降低大黄蒽醌的含量。
综上所述，通过上述实施例实验证明，采用水提方式能够降低大黄蒽醌类成分的提取率；提取没食子酸部位的乙酸乙酯萃取方式不仅可以富集纯化没食子酸，同样能够降低提取物中大黄蒽醌类成分的含量。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而这些属于本发明的实质精神所引伸出的显而易见的变化或变动仍属于本发明的保护范围。
Claims (1)
1.一种大黄提取物的制备方法，其特征在于，包括以下步骤：
①将熟大黄药材粉碎成粗粉，用水加热回流提取，滤过，合并滤液；
②将合并的滤液减压浓缩，得水提浓缩液，放冷；
③加入乙醇，醇沉，醇沉物备用；
④醇沉上清液减压回收乙醇至无醇味，得醇提浓缩液；
⑤醇提浓缩液用乙酸乙酯萃取，合并乙酸乙酯层萃取液，回收乙酸乙酯后，与醇沉物混合均匀，减压干燥，粉碎，得大黄提取物，所述的步骤①，大黄原料与水之比为1：6-1：10；提取次数为2-4次；提取时间1-2小时，所述的步骤②，水提浓缩液的密度在60℃时为1.10-1.15g/ml,所述的步骤③，乙醇加入量为浓缩液体积的2-6倍量，醇沉时间为12-36小时，所述的步骤④，醇提浓缩液的密度在60℃时为1.10-1.15g/ml，所述的步骤⑤，乙酸乙酯每次用量为醇提浓缩液体积的1-3倍，萃取次数为2-6次。
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| 水提-醇沉法提取大黄多糖工艺优化研究;孙莹等;《中国实用医药》;20100630;第5卷(第18期);6-8 * |
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