水提醇沉的要求

水提的浓缩物要醇沉有什么要求?
2025-02-19 19:10:18
推荐回答(2个)
回答1:

水提醇沉淀法(水醇法):先以水为溶媒提取药材有效成分,再用乙醇沉淀除去杂质的方法。利用水、乙醇对有效成分和无效成分溶解度的不同使之分离精制。

(一) 工艺依据:通常含醇量 50~60%时淀粉、多糖沉淀。60%或70%以上,除鞣质、树脂外,大部分被除掉。

(二) 操作

中药,加水煎2~3次,过滤,滤液浓缩至1:1~1:2(ml:g)或相对密度1.08-1.15,

加适量乙醇,使含醇量达一定要求(50~60%,60~70%)冷藏(10~48小时),滤过。

(三) 影响因素

1.醇沉浓度的选择

一般45%醇沉可去淀粉、糊精等无效成分,50%醇沉后制颗粒、片、胶囊较多;60~70%醇沉制合剂、口服液,澄清度好。50~60%、70~80%二次醇沉多用在注射液、滴眼液等,而60~80%的沉淀经丙酮等洗涤后,可得多糖。

2.所用乙醇浓度的选择

根据经验,乙醇的浓度与药液需要达到的乙醇浓度之间差20%~25%最佳。浓度太低,乙醇用量大浪费,回收不方便,且沉淀成絮状,难以下沉,效果差;浓度太高,得到的醇提液较少,沉淀中含有大量的有效物质,且加入高浓度乙醇,易造成局部浓度过高,形成大块沉淀,将有效成分包裹,随沉淀除去。

3.药液浓度

药液浓缩后的相对密度如果太小,由于药液比较稀,形成的沉淀不易聚结,难以下沉,且浪费乙醇;如相对密度太大,药液因长时间煎煮浓缩,易使苷类、萜类、维生素等成分破坏,且造成淀粉糊化,醇沉时形成大块,包裹有效成分。

4.药液温度

药液温度高,遇冷的乙醇后,骤冷易聚结成团状沉淀,且沉淀增长很快,防碍了有效物质的提出,故效果不理想;药液温度低,相对难以导致沉淀聚结,效果最佳。一般浓缩后放冷至室温。

5.加醇方式

加醇应采用慢加快搅的方法,以使加入的乙醇迅速分散,避免局部浓度过高,形成大块沉淀。且应按一个方向搅动,以免使药液乳化,不易使沉淀下沉分层。如用来醇沉的乙醇浓度不等,应按浓度从小到大的顺序加入。

(四)操作要点

1 药液浓缩:减压低温浓缩;浓缩前后可调节pH,以保留有效成分,如生物碱在酸性下溶解;浓缩程度适宜,浓度太高,易使水溶性低的成分损失(苷元、香豆精)。

2 加醇方式:慢加快搅逐步提高醇浓度。分次醇沉或以梯度递增方式逐步提高乙醇浓度的方法进行醇沉(有利于除杂,减少杂质对有效成分包裹)。

3 醇用量的计算

乙醇用量计算公式: C2*(V+X)=C1*X

对同一品种可用回收乙醇作第二次沉淀,注意回收乙醇浓度有变化,一般在80~85%,精馏达90%以上,须计算后加入或再补加浓乙醇。

4 冷藏与处理:含醇药液慢慢降至室温时,移至冷库于5~10℃静置冷藏(不能结冰,杂质易停留在晶格中不易沉淀)。滤过时,吸取上清夜滤过,下层沉淀慢慢滤过。

6.醇沉是很实用的技术,沉淀会包裹有效成分,增加洗涤可增加有效成分的转移率。

7.与之相适应的纯水法除淀粉和粘液质等,很少用,不太合理。

回答2:

坦白地说这题我不会

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