CN115227741A - 一种肉苁蓉提取物纯化方法及设备 - Google Patents
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Abstract
本发明涉中药精加工领域,具体涉及一种肉苁蓉提取物纯化方法,包括将肉苁蓉经过粉碎、利用提取溶剂进行浸提,过滤回收滤液;用预处理过的大孔吸附树脂装填玻璃柱,用蒸馏水饱和,将滤液常压过柱后,减压浓缩至原体积的1/3‑1/2的浓缩液;向浓缩液中加入体积分数为95%的乙醇,进行醇沉,过滤得沉淀物以及二次滤液;对二次滤液进行纳滤,即将二次滤液通过纳滤膜,回收乙醇滤出液,并将截留液重新作为提取溶剂使用;本发明对消耗溶剂进行了有效回收利用,大大降低了纯化成本。
Description
技术领域
本发明涉中药精加工领域,具体涉及一种肉苁蓉提取物纯化方法及纯化设备。
背景技术
肉苁蓉为列当科多年生寄生植物,主要分布于内蒙古、宁夏、甘肃、新疆、青海等沙漠、荒漠干旱地带,具有极高的药用价值,有“沙漠人参”之美誉,是我国传统的名贵中药材。肉苁蓉中含有丰富的肉苁蓉多糖、苯乙醇苷、生物碱、有机酸等,此外,还含有大量的矿物元素。肉苁蓉有补肾助阳,润肠通便之功效;用于治疗肾阳亏虚,精血不足之阳痿早泄、宫冷不孕、腰膝酸痛、疲软无力,以及肠燥津枯之便秘等症。《本草求真》中记有:“肉苁蓉,诸书既言峻补精血,又言力能兴阳助火,是明因其气温,力专滋阴,得此阳随阴附,而阳自见兴耳。惟其力能滋补,故凡症痕积块,得此而坚即消。惟其滋补而阳得助,故凡遗精茎痛,寒热时作,亦得因是而除。”近代药理学研究表明,肉苁蓉多糖能提高机体免疫功能,促进DNA合成,增强体力,提高智力,具有明显的抗衰老作用。
在现有的研究中,肉苁蓉中有效成分可以经过萃取以及纯化,传统萃取技术包括溶剂浸提法、超声波萃取、微波萃取等,肉苁蓉中多糖采用醇沉技术获得,而苯乙醇苷等成分纯化的经典方法主要是利用不同理化性质上的差异进行分离,主要包括有机溶剂萃取、沉淀、结晶及层析分离等方法。问题在于上述方法存在生产周期长、消耗溶剂较多和耗能较大的缺点,并不适用于工业生产。
发明内容
有鉴于此,本发明的目的是克服现有技术中的缺陷,提供一种肉苁蓉提取物纯化方法,对消耗溶剂进行了有效回收利用。
本发明的一种肉苁蓉提取物纯化方法,包括以下步骤:
(1)将肉苁蓉经过粉碎、利用提取溶剂进行浸提,过滤回收滤液;
(2)用预处理过的大孔吸附树脂装填玻璃柱,用蒸馏水饱和,将滤液常压过柱后,减压浓缩至原体积的1/3-1/2的浓缩液;
(3)向浓缩液中加入体积分数为95%的乙醇,进行醇沉,过滤得沉淀物以及二次滤液;
(4)对二次滤液进行纳滤,即将二次滤液通过纳滤膜,回收乙醇滤出液,并将截留液重新返回步骤(1)作为提取溶剂使用。
步骤(1)所述的提取溶剂含有体积分数0%-50%的乙醇。
步骤(4)所述的纳滤膜,膜截留分子量为100-200Da,操作压力操作压力1-10bar,温度控制为常温,滤出液即为乙醇,截留液含有多糖以外的有效成分。
所述浸提的具体过程还包括利用乙醇滤出液对肉苁蓉进行前处理浸提,前处理浸提的提取液通过大孔树脂,收集洗脱液,浓缩、干燥。
上述方法在以下结构的设备中完成,该设备包括浸提罐、一次过滤器、大孔树脂柱、浓缩罐、醇沉罐、二次过滤器以及纳滤罐,肉苁蓉原料在浸提罐中浸提后经过一次过滤器获得滤液,滤液经过一次过滤器的出口进入大孔树脂柱进行除杂,除杂后进入浓缩罐,浓缩液一次进入醇沉罐以及二次过滤器,在二次过滤器中分离沉淀物以及二次滤液,二次滤液进入纳滤罐,截留液重新返回浸提罐。
所述纳滤罐的滤出液出口连接至浸提罐的入口,所述一次过滤器还连接有第二大孔树脂柱。
本发明的有益效果是:本发明公开的一种肉苁蓉提取物纯化方法,采用提取溶剂对肉苁蓉进行浸提,采用醇沉方式纯化获得肉苁蓉多糖提取物,并且利用纳滤对乙醇进行回收,乙醇滤出液以及含水截留液均可被用作再次提取纯化的试剂,大大降低了溶剂的消耗。
附图说明
下面结合附图和实施例对本发明作进一步描述:
图1为本发明中纯化设备的结构框图。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅是本发明的一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
如图1所示,本实施例中的肉苁蓉提取物纯化过程在纯化设备中完成,该纯化设备暴包括浸提罐、一次过滤器、大孔树脂柱、浓缩罐、醇沉罐、二次过滤器以及纳滤罐,首先将肉苁蓉进行粉碎,加入浸提罐中,并向浸提罐中加入纯水作为提取溶剂,水的用量为肉苁蓉质量的10-12倍,例如若采用新鲜肉苁蓉可采用10倍纯水,干制品肉苁蓉即可采用12被纯水作为提取溶剂,将混合物在加热的状态下进行浸提,可以辅以微波或超声波加快提取速度。
浸提完成后将混合物通入一次过滤器,过滤得滤液和滤渣,将滤渣重复进行浸提2-3次,合并滤液,将滤液通过由预处理过的大孔吸附树脂制得的大孔树脂柱进行除杂,且大孔树脂柱预先用蒸馏水饱和,将滤液常压过柱后,加入浓缩罐,减压浓缩至原体积的1/3-1/2的浓缩液。
大孔吸附树脂型号为HPD-400、HPD-450、HPD-600、HPD-750、HPD-826、DM-130、ADS-17中的一种。
浓缩液仅管道进入醇沉罐,向浓缩液中加入体积分数为95%的乙醇,并进行搅拌混合,至整体乙醇体积分数不低于80%,通过静置或离心使多糖沉淀物完全沉淀下来,通过二次过滤器分离二次滤液以及沉淀物,沉淀物经过清洗、烘干得纯化后的多糖。
二次滤液含大量乙醇以及少量多糖、大量苯乙醇苷等其他有效成分,将其通入纳滤罐进行回收,纳滤罐中设置有纳滤膜,纳滤膜膜截留分子量为100-200Da,操作压力1-10bar,温度控制为常温,滤出液即为乙醇,将滤出液适度蒸馏浓缩后作为醇沉部分的原料,而截留液则可以作为提取溶剂返回到浸提罐中。
实施例2
本实施例与实施例一的区别在于不再采用纯水作为提取溶剂,而是直接采用最终步骤的截留液作为提取溶剂,在浸提之前对截留液进行处理,保证其乙醇浓度在0-50%,方便提取多糖,而乙醇滤出液不再作为醇沉原料,而是在蒸馏浓缩提纯后,对肉苁蓉进行前处理浸提,即在提取溶剂加入之前先提取一次,将前处理浸提的提取液通过大孔树脂,收集洗脱液,浓缩、干燥,得到苯乙醇苷纯化物。
上述过程前处理浸提在浸提罐中完成,经过一次过滤器后得到前处理浸提的提取液以及滤渣,前处理浸提的提取液加入到第二大孔树脂柱中进行纯化,滤渣则可以返回浸提罐中。
最后说明的是,以上实施例仅用以说明本发明的技术方案而非限制,尽管参照较佳实施例对本发明进行了详细说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的宗旨和范围,其均应涵盖在本发明的权利要求范围当中。
Claims (8)
1.一种肉苁蓉提取物纯化方法,其特征在于:包括以下步骤:
(1)将肉苁蓉经过粉碎、利用提取溶剂进行浸提,过滤回收滤液;
(2)用预处理过的大孔吸附树脂装填玻璃柱制成大孔树脂柱,用蒸馏水饱和,将滤液常压过柱后,减压浓缩至原体积的1/3-1/2的浓缩液;
(3)向浓缩液中加入体积分数为95%的乙醇,进行醇沉,过滤得沉淀物以及二次滤液;
(4)对二次滤液进行纳滤,即将二次滤液通过纳滤膜,回收乙醇滤出液,并将截留液重新返回步骤(1)作为提取溶剂使用。
2.根据权利要求1所述的一种肉苁蓉提取物纯化方法,其特征在于:步骤(1)所述的提取溶剂含有体积分数0%-50%的乙醇。
3.根据权利要求1所述的一种肉苁蓉提取物纯化方法,其特征在于:所述浸提的具体过程至少包括向肉苁蓉原料中加入提取溶剂加热提取,提取溶剂的用量为肉苁蓉重量的10-12倍,且提取次数为2-3次。
4.根据权利要求3所述的一种肉苁蓉提取物纯化方法,其特征在于:所述浸提的具体过程还包括利用乙醇滤出液对肉苁蓉进行前处理浸提,前处理浸提的提取液通过大孔树脂,收集洗脱液,浓缩、干燥。
5.根据权利要求4所述的一种肉苁蓉提取物纯化方法,其特征在于:步骤(2)所述的大孔吸附树脂型号为HPD-400、HPD-450、HPD-600、HPD-750、HPD-826、DM-130、ADS-17中的一种。
6.根据权利要求1所述的一种肉苁蓉提取物纯化方法,其特征在于:步骤(4)所述的纳滤膜,膜截留分子量为100-200Da,操作压力操作压力1-10bar,温度控制为常温。
7.一种肉苁蓉提取物纯化设备,采用权利要求1-6中任意一项所述的方法对肉苁蓉提取物进行纯化,其特征在于:包括浸提罐、一次过滤器、大孔树脂柱、浓缩罐、醇沉罐、二次过滤器以及纳滤罐,肉苁蓉原料在浸提罐中浸提后经过一次过滤器获得滤液,滤液经过一次过滤器的出口进入大孔树脂柱进行除杂,除杂后进入浓缩罐,浓缩液一次进入醇沉罐以及二次过滤器,在二次过滤器中分离沉淀物以及二次滤液,二次滤液进入纳滤罐,截留液重新返回浸提罐。
8.根据权利要求7所述的一种肉苁蓉提取物纯化设备,其特征在于:所述纳滤罐的滤出液出口连接至浸提罐的入口,所述一次过滤器还连接有第二大孔树脂柱。
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