CN110025645B - 一种提取西洋参总皂苷的方法 - Google Patents
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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, decoction
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Abstract
本发明公开了一种提取西洋参总皂苷的方法,该方法采用食盐水溶液浸煮干燥粉碎的西洋参根须,然后经脱色处理、复合树脂柱层析、浓缩、萃取、浓缩得西洋参总皂苷粗品,粗品再经过柱层析、重结晶等步骤,获得杂质含量少的西洋参总皂苷产品,本发明具有方法简单、成本低、收率高、生产周期短、色素少的特点,适用于工业化生产和市场推广应用。
Description
技术领域
本发明涉及一种从干燥西洋参根须中提取西洋参总皂苷的工业化生产方法。
背景技术
西洋参(Panax quinquefolius)是五加科人参属多年生草木植物,别名花旗参、洋参、西洋人参,原产于加拿大的大魁北克与美国的威斯康辛州,中国北京怀柔与长白山等地也有种植。加拿大产的叫西洋参,美国参产的叫花旗参。
西洋参中主要成分为人参皂苷,已分离出的5种皂苷分别为:人参皂苷R0、Rb1、Rg1、Re和假人参皂苷F11;西洋参所含有效成分与人参单体皂苷类别基本相同,甚至所含皂苷元也完全一致,均系齐墩果酸、人参二醇和人参三醇;但由于人参二醇单体皂苷的Rb1的含量高于人参,因此,形成二者疗效和应用上的差异,各有特色不可互相替代。
西洋参总皂苷是西洋参中最主要的有效成分之一,也是生理活性最显著的物质;迄今为止,人们已经在西洋参中提取了多种皂苷单体;西洋参总皂苷单体的种类虽然不少,但主要是三萜类化合物,与人参皂苷结构有相似之处,但有些是西洋参所独有的。西洋参总皂苷可以分为三大类群:Ra组、Rb组(包括Ro、Ra1、Ra2、Ra3、Rb1、Rb2、Rb3、Rc、Rd等几个亚型)和Rg组(包括Re、Rg1、Rg2、Rg3、Rh1、Rh2六个亚型)。相关研究表明,在这三大类群中,Ra组的几种单体生理活性较弱,而Rb组和Rg组的生理活性相对较强;有研究把西洋参与人参作对比,西洋参中的西洋参总皂苷以及人参皂苷r64的含量明显高于同剂量人参的皂苷含量,由此说明为什么西洋参被列为名贵中药;
西洋参皂甙具有抗缺氧、抗疲劳和抗衰老作用,可改善和增强记忆力,西洋参具有双向调节免疫调节作用,降脂以及具有抗心律失常、抗心肌缺血和再灌损伤等的作用;西洋参多糖具有抗癌及提高免疫力的功效。
从干燥西洋参根须中提取西洋参总皂苷的现有技术或传统方法中存在如下问题:
(1)目前,西洋参总皂苷的规模化生产中采用的基本是常规的提取工艺,这些方法不同程度上存在着提取时间长,效率低;
(2)传统方法提取所得总皂苷含量为50~80%,没有更高含量总皂苷提取物,即使得到高含量的西洋参总皂苷也要经过多次柱层析,成本较高;
(3)西洋参原料资源有限,而人工合成西洋参总皂苷并未取得理想的效果,在资源有限、人工合成并不完善的情况下,迫切需要一些能提取到西洋参总皂苷的资源支撑。
发明内容
本发明目的在于提供一种提取西洋参总皂苷的方法,该方法清洁、价格低廉、提取条件不苛刻、副产物较少、色素少、提取收率较高,方法简单可控,生产周期短,适合工业化生产西洋参总皂苷。
本发明的目的通过如下技术方案实现:
(1)以干燥的西洋参须根为原料,经粉碎后,在原料粉中加入其质量4~6倍的食盐水在40~60℃下浸煮,过滤;滤渣加食盐水,再浸煮1~2次,收集合并滤液;
所述粉碎后的原料粒径为10~20目;食盐水的质量浓度为10%~15%;
(2)按每1kg活性炭-硅藻土混合物加入60~80kg滤液的比例,将滤液加入到活性炭-硅藻土混合物柱中进行脱色及除杂,利用活性炭和硅藻土吸附西洋参总皂苷提取液中的色素及其他杂质,滤液加完后,用水冲洗柱子,冲洗2~4个柱体积,收集洗出液;
所述活性炭-硅藻土混合物中活性炭和硅藻土的质量比为1~2:1,活性炭和硅藻土的粒径均为80~100目;
(3)按每1kg ADS-7和KLIEC-Aw树脂混合物添加40~60kg洗出液的比例,将洗出液加入到上述两种混合树脂柱中吸附西洋参总皂苷,利用树脂吸附西洋参总皂苷,完成吸附后加入甲醇或乙醇解析西洋参总皂苷,收集甲醇或乙醇洗脱液,减压浓缩抽干得西洋参总皂苷粗提物;
所述ADS-7和KLIEC-Aw树脂混合物中ADS-7树脂和KLIEC-Aw树脂的质量比为1:1~3;
(4)将西洋参总皂苷粗提物用正丁醇或/和异戊醇溶解,待其溶清后,加入有机溶剂体积0.25~0.5倍的水萃取,充分静置2~4h,分层,分出有机相,在水相中再加入相同有机溶剂萃取1~2次,充分静置,分出有机相;合并有机相并在60~70℃、减压条件下浓缩得到西洋参总皂苷粗品;
所述西洋参总皂苷粗提物:正丁醇或/和异戊醇g:mL为1:15~20;
(5)将西洋参总皂苷粗品用甲醇水溶液溶解后,拌料胶,干燥后加入到硅胶(200~300目)、中性氧化铝(200~300目)或酸性氧化铝(200~300目)柱中进行柱层析,用氯仿-乙酸乙酯-水混合液或氯仿-丙酮-水混合液洗脱,TLC监控,收集含有西洋参总皂苷的洗脱液,减压浓缩干燥后,得西洋参总皂苷半成品;
所述甲醇水溶液是甲醇和水按体积比100:1的比例混合制得;拌料的料胶质量比为1: 1.0~1.2,装柱时料胶质量比为1:20~25;氯仿-乙酸乙酯-水混合液中氯仿:乙酸乙酯:水=4~6:1:0.1,氯仿-丙酮-水混合液中氯仿:丙酮 :水=7~9:1:0.1;
(6)将西洋参总皂苷半成品用甲醇-丙酮-水混合液或四氢呋喃-丙酮-水混合液在60~70℃下回流溶解,冷却至室温,-10~0℃下冷冻结晶8~10h,减压抽滤;晶体再用相同方法重结晶1次,减压抽滤;晶体干燥,即得西洋参总皂苷;
其中西洋参总皂苷半成品:甲醇:丙酮:水=1g:2~3mL:2~3mL:0.2~0.3mL,西洋参总皂苷半成品: 四氢呋喃:丙酮:水=1g:3~4mL:1~2mL:0.1~0.2mL。
本发明优点和技术效果:
(1)本发明利用盐水的高渗透压,浸煮西洋参,西洋参细胞在高渗透压作用下,西洋参总皂苷能快速且最大程度的被提取出来,大大提高西洋参总皂苷的收率;方法简单可行、成本低、收率高,适合工业化生产;
(2)本发明通过活性炭及硅藻土混合物脱色,可以保证西洋参总皂苷不被吸附,且达到吸附脱除色素及部分水溶剂杂质;使西洋参总皂苷含量迅速富集;方法简单可行、成本低、收率高,适合工业化生产;
(3)本发明通过用正丁醇或异戊醇溶解,加水萃取,可以保留西洋参总皂苷,同时除去大量水溶解杂质,保证了西洋参总皂苷含量快速提高,减轻后序工作的压力,方法简单可行,生产成本低,适合工业化生产;
(4)本发明通过ADS-7吸附树脂和KLIEC-Aw树脂的混合利用,快速吸附目标物且吸附量较大,同时除去大量杂质,提高了目标物的含量;再经过一次正相柱层析,目标物含量从8%提高到至90%以上;方法简单可行,生产成本低,适合工业化生产;
(5)本发明通过甲醇-丙酮-水混合液或四氢呋喃-丙酮-水混合液加热回流溶解、冷冻结晶等方法,能使西洋参总皂苷含量提高至98%以上,质量好、收率高,方法简单可行,操作可控,回收液可以重复利用,生产成本低、适合工业化生产。
具体实施方式
下面通过实施例对本发明作进一步详细说明,但本发明保护范围不局限于所述内容。
实施例1:本提取西洋参总皂苷的方法如下:
(1)以50kg干燥的西洋参须根为原料,粉碎至10-20目后,在原料粉中加入其质量6倍的质量浓度为10%食盐水在40℃下浸煮,过滤;滤渣加食盐水,再浸煮1次,收集合并滤液;
(2)按每1kg活性炭-硅藻土混合物加入60kg滤液的比例,将滤液加入到活性炭-硅藻土混合物(80目活性炭和100目硅藻土的质量比为1:1)柱中进行脱色及除杂,利用活性炭和硅藻土吸附西洋参总皂苷提取液中的色素及其他杂质,滤液加完后,用水冲洗柱子,冲洗2个柱体积,收集洗出液;
(3)按每1kg ADS-7和KLIEC-Aw树脂混合物(质量比为1:2)添加40kg洗出液的比例,将洗出液加入到上述两种混合树脂柱中吸附西洋参总皂苷,利用树脂吸附西洋参总皂苷,完成吸附后加入甲醇解析西洋参总皂苷,收集甲醇洗脱液,减压浓缩抽干得西洋参总皂苷粗提物,含量为12.5%;
(4)将西洋参总皂苷粗提物用正丁醇溶解,其中西洋参总皂苷粗提物:正丁醇g:mL为1:15,待其溶清后,加入正丁醇体积0.25倍的水萃取,充分静置2h,分层,分出有机相,在水相中再加入正丁醇萃取1次,充分静置2h,分出有机相;合并有机相并在60℃、减压条件下浓缩得到西洋参总皂苷粗品;
(5)将西洋参总皂苷粗品用甲醇水(体积比100:1)溶液溶解后,拌料胶,料胶质量比为1: 1.0;干燥后加入到硅胶(200~300目)柱中进行柱层析,装柱时料胶质量比为1:20,用氯仿-乙酸乙酯-水混合液(5:1:0.1)洗脱,TLC监控,收集含有西洋参总皂苷的洗脱液,减压浓缩干燥后,得西洋参总皂苷半成品;
(6)将西洋参总皂苷半成品用甲醇-丙酮-水混合液在60℃下回流溶解,其中西洋参总皂苷半成品:甲醇:丙酮:水=1g:2mL:2mL:0.3mL,冷却至室温,-10℃下冷冻结晶8h,减压抽滤;晶体再加入甲醇-丙酮-水混合液回流溶解,-10℃下冷冻结晶8h,减压抽滤;晶体干燥,即得西洋参总皂苷,含量为98.5%,收率87.8%。
实施例2:本提取西洋参总皂苷的方法如下:
(1)以50kg干燥的西洋参须根为原料,粉碎至10-20目后,在原料粉中加入其质量5倍的质量浓度为12%食盐水在50℃下浸煮,过滤;滤渣加食盐水,再浸煮2次,收集合并滤液;
(2)按每1kg活性炭-硅藻土混合物加入80kg滤液的比例,将滤液加入到活性炭-硅藻土混合物(100目活性炭和100目硅藻土的质量比为2:1)柱中进行脱色及除杂,利用活性炭和硅藻土吸附西洋参总皂苷提取液中的色素及其他杂质,滤液加完后,用水冲洗柱子,冲洗3个柱体积,收集洗出液;
(3)按每1kg ADS-7和KLIEC-Aw树脂混合物(质量比为1:1)添加60kg洗出液的比例,将洗出液加入到上述两种混合树脂柱中吸附西洋参总皂苷,利用树脂吸附西洋参总皂苷,完成吸附后加入甲醇解析西洋参总皂苷,收集甲醇洗脱液,减压浓缩抽干得西洋参总皂苷粗提物,含量为11.6%;
(4)将西洋参总皂苷粗提物用异戊醇溶解,其中西洋参总皂苷粗提物: 异戊醇g:mL为1:18,待其溶清后,加入异戊醇体积0.4倍的水萃取,充分静置3h,分层,分出有机相,在水相中再加入异戊醇萃取1次,充分静置2h,分出有机相;合并有机相并在65℃、减压条件下浓缩得到西洋参总皂苷粗品;
(5)将西洋参总皂苷粗品用甲醇水(体积比100:1)溶液溶解后,拌料胶,料胶质量比为1: 1.2;干燥后加入到中性氧化铝(200~300目)柱中进行柱层析,装柱时料胶质量比为1:22,用氯仿-乙酸乙酯-水混合液(4:1:0.1)洗脱,TLC监控,收集含有西洋参总皂苷的洗脱液,减压浓缩干燥后,得西洋参总皂苷半成品;
(6)将西洋参总皂苷半成品用甲醇-丙酮-水混合液在65℃下回流溶解,其中西洋参总皂苷半成品:甲醇:丙酮:水=1g:3mL:2mL:0.2mL,冷却至室温,-5℃下冷冻结晶9h,减压抽滤;晶体再加入甲醇-丙酮-水混合液回流溶解,-5℃下冷冻结晶9h,减压抽滤;晶体干燥,即得西洋参总皂苷,含量为98.6%,收率89.5%。
实施例3:本提取西洋参总皂苷的方法如下:
(1)以50kg干燥的西洋参须根为原料,粉碎至10-20目后,在原料粉中加入其质量6倍的质量浓度为15%食盐水在60℃下浸煮,过滤;滤渣加食盐水,再浸煮1次,收集合并滤液;
(2)按每1kg活性炭-硅藻土混合物加入70kg滤液的比例,将滤液加入到活性炭-硅藻土混合物(90目活性炭和80目硅藻土的质量比为1.5:1)柱中进行脱色及除杂,利用活性炭和硅藻土吸附西洋参总皂苷提取液中的色素及其他杂质,滤液加完后,用水冲洗柱子,冲洗4个柱体积,收集洗出液;
(3)按每1kg ADS-7和KLIEC-Aw树脂混合物(质量比为1:3)添加50kg洗出液的比例,将洗出液加入到上述两种混合树脂柱中吸附西洋参总皂苷,利用树脂吸附西洋参总皂苷,完成吸附后加入甲醇解析西洋参总皂苷,收集甲醇洗脱液,减压浓缩抽干得西洋参总皂苷粗提物,含量为13.1%;
(4)将西洋参总皂苷粗提物用正丁醇和异戊醇溶解,其中西洋参总皂苷粗提物:正丁醇: 异戊醇g:mL:mL为1:10:10,待其溶清后,加入正丁醇体积0.5倍的水萃取,充分静置4h,分层,分出有机相,在水相中再加入正丁醇萃取2次,充分静置2h,分出有机相;合并有机相并在70℃、减压条件下浓缩得到西洋参总皂苷粗品;
(5)将西洋参总皂苷粗品用甲醇水(体积比100:1)溶液溶解后,拌料胶,料胶质量比为1: 1.1;干燥后加入到酸性氧化铝(200~300目)柱中进行柱层析,装柱时料胶质量比为1:25,用氯仿-丙酮-水混合液(8:1:0.1)洗脱,TLC监控,收集含有西洋参总皂苷的洗脱液,减压浓缩干燥后,得西洋参总皂苷半成品;
(6)将西洋参总皂苷半成品用四氢呋喃-丙酮-水混合液在70℃下回流溶解,其中西洋参总皂苷半成品: 四氢呋喃:丙酮:水=1g:3mL:2mL:0.1mL,冷却至室温,0℃下冷冻结晶10h,减压抽滤;晶体再加入四氢呋喃-丙酮-水混合液回流溶解,-5℃下冷冻结晶9h,减压抽滤;晶体干燥,即得西洋参总皂苷,含量为98.2%,收率87.9%。
Claims (3)
1.一种提取西洋参总皂苷的方法,其特征在于按以下步骤进行:
(1)以干燥的西洋参须根为原料,经粉碎后,在原料粉中加入其质量4~6倍的食盐水在40~60℃下浸煮,过滤;滤渣加食盐水,再浸煮1~2次,收集合并滤液;
(2)按每1kg活性炭-硅藻土混合物加入60~80kg滤液的比例,将滤液加入到活性炭-硅藻土混合物柱中进行脱色及除杂;用水冲洗柱子,冲洗2~4个柱体积,收集洗出液;
(3)按每1kg ADS-7和KLIEC-Aw树脂混合物添加40~60kg洗出液的比例,将洗出液加入到上述两种混合树脂柱中吸附西洋参总皂苷,完成吸附后加入甲醇或乙醇解析西洋参总皂苷,收集甲醇或乙醇洗脱液,减压浓缩抽干得西洋参总皂苷粗提物;
(4)将西洋参总皂苷粗提物用正丁醇或/和异戊醇溶解,待其溶清后,加入有机溶剂体积0.25~0.5倍的水萃取,充分静置2~4h,分层,分出有机相,在水相中再加入相同有机溶剂萃取1~2次,充分静置,分出有机相;合并有机相并在60~70℃、减压条件下浓缩得到西洋参总皂苷粗品;
(5)将西洋参总皂苷粗品用甲醇水溶液溶解后,拌料胶,干燥后加入到硅胶、中性氧化铝或酸性氧化铝柱中进行柱层析,用氯仿-乙酸乙酯-水混合液或氯仿-丙酮-水混合液洗脱,TLC监控,收集含有西洋参总皂苷的洗脱液,减压浓缩干燥后,得西洋参总皂苷半成品;
(6)将西洋参总皂苷半成品用甲醇-丙酮-水混合液或四氢呋喃-丙酮-水混合液在60~70℃下回流溶解,冷却至室温,-10~0℃下冷冻结晶8~10h,减压抽滤;晶体再用相同方法重结晶1次,减压抽滤;晶体干燥,即得西洋参总皂苷;
所述食盐水的质量浓度为10%~15%;
所述活性炭-硅藻土混合物中活性炭和硅藻土的质量比为1~2:1,活性炭和硅藻土的粒径均为80~100目;
所述ADS-7和KLIEC-Aw树脂混合物中ADS-7树脂和KLIEC-Aw树脂的质量比为1:1~3;
氯仿-乙酸乙酯-水混合液中氯仿:乙酸乙酯:水=4~6:1:0.1,氯仿-丙酮-水混合液中氯仿:丙酮 :水=7~9:1:0.1;
步骤(6)中西洋参总皂苷半成品:甲醇:丙酮:水=1g:2~3mL:2~3mL:0.2~0.3mL,西洋参总皂苷半成品: 四氢呋喃:丙酮:水=1g:3~4mL:1~2mL:0.1~0.2mL。
2.根据权利要求1所述的提取西洋参总皂苷的方法,其特征在于:步骤(4)中西洋参总皂苷粗提物:正丁醇或/和异戊醇g:mL为1:15~20。
3.根据权利要求1所述的提取西洋参总皂苷的方法,其特征在于:甲醇水溶液是甲醇和水按体积比100:1的比例混合制得。
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