CN109528804B - 一种太子参环肽提取物的制备方法 - Google Patents
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Abstract
本发明公开了一种太子参环肽提取物的制备方法，其包括太子参的提取、脱脂、除氨基酸、醇沉及冻干的步骤。按本发明方法进行制备，所得提取物中总环肽含量在95%以上，可用于开发太子参环肽类成分的保健品，促进太子参深加工产品的发展。
Description
技术领域
本发明属于天然活性成分制备领域，具体涉及一种太子参环肽提取物的制备方法。
背景技术
太子参为石竹科植物孩儿参Pseudostellaria heterophylla （Miq.）Pax ex Paxet Hoffm.的干燥块根。为我国传统中药，其味甘、微苦，平，归脾、肺经，具有益气健脾，生津润肺之功效，用于脾虚体倦，食欲不振，病后虚弱，气阴不足，自汗口渴，肺燥干咳。
现有研究表明。太子参中含有多糖、环肽、皂苷等成分，具有抗疲劳、抗缺氧、抗应激、抗衰老等药理作用，其中，环肽类成分是其特征成分。为推动太子参行业发展，开发太子参环肽类成分的相关功能产品及保健品，如何有效获得含太子参环肽类成分的提取物已成为亟待解决的问题之一。
发明内容
本发明的目的在于提供一种太子参环肽提取物的制备方法，其所得提取物中总环肽含量在95%以上。
为实现上述目的，本发明采用如下技术方案：
一种太子参环肽提取物的制备方法，其包括以下步骤：
1）提取：将太子参粉碎，过三号筛，按料液比1:20 g/mL加入乙酸乙酯，于90℃索氏提取4h，然后将提取液冷却至室温，旋蒸去除溶剂，得太子参乙酸乙酯提取物；
2）脱脂：将太子参乙酸乙酯提取物置于循环超声波提取机中，按料液比1:20 g/mL加入石油醚进行超声脱脂，然后抽滤，所得滤渣重复石油醚脱脂3次后，挥干溶剂，再按料液比1:20 g/mL加入无水乙醇，60℃超声提取1 h，然后抽滤，滤液冷却至室温后旋蒸去除溶剂；
3）除氨基酸：将步骤2）脱脂后的残渣用热水充分溶解后，按体积比1:2加入乙酸乙酯，萃取3次，所得乙酸乙酯萃取相浓缩至干后，重新溶解于热水中，再按体积比1:1加入水饱和正丁醇，萃取3次，所得正丁醇相按体积比1:1加入40 vol%的氨试液，萃取3次，然后弃去氨试液，收集正丁醇相浓缩至干，所得残渣继续溶解于热水中，再按体积比1:1加入氯仿，萃取3次，所得氯仿相减压浓缩至干；
4）醇沉：将步骤3）所得残渣加无水乙醇溶解后，静置12h，抽滤，收集滤液；
5）冻干：将步骤4）所得滤液加水配成50vol%醇溶液，于-80℃预冷冻后进行冷冻干燥，即得太子参环肽提取物，其总环肽含量在92%以上。
本发明的显著优点在于：本发明提供了一种太子参环肽提取物的制备方法，以此方法制得的提取物中总环肽含量在95%以上，可用于开发太子参环肽类成分的保健品。
附图说明
图1为依据太子参乙酸乙酯提取物的HPLC指纹图谱进行制备的流程示意图。
图2为所制备的太子参环肽提取物中环肽群的HPLC色谱图。
具体实施方式
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
仪器和试剂
1.1仪器
Waters2695高效液相色谱仪(美国Waters公司)，Waters2998二极管检测器（美国Waters公司），Hypersil ODS分析色谱柱（4.6mm×250mm，5μm，大连依利特分析仪器有限公司），循环超声波提取机（北京弘祥隆生物技术有限公司），真空冷冻干燥机（美国ThermoFisher仪器有限公司，型号：RVT4104-230），BUCHI R-100旋转蒸发仪（瑞士BUCHI公司），恒温水浴锅（上海精宏实验设备有限公司）。
材料
药材：太子参
色谱纯试剂：乙腈（批号：179156，美国Fisher试剂公司），甲醇（批号：10887607718，德国默克试剂公司），磷酸（批号：167217，美国Fisher试剂公司）；
分析纯试剂：石油醚（批号：1810301，西陇科学股份有限公司出品），乙酸乙酯（批号：1809131，西陇科学股份有限公司出品），乙醇（批号：18100902，西陇科学股份有限公司出品），正丁醇（批号：1808121，西陇科学股份有限公司出品），氨水（批号：1810405，西陇科学股份有限公司出品），氯仿（批号：1810585，西陇科学股份有限公司出品），水为电阻率为18.2Ω的超纯水。
溶液的配制
40%氨试液的配制：量取氨水200mL，置500mL烧杯中，加入300mL蒸馏水，混匀，既得40%氨试液。
水饱和正丁醇的配制：量取正丁醇500mL，置1000mL分液漏斗中，加入500 mL蒸馏水，振摇，放置24h后，取正丁醇层，既得水饱和正丁醇溶液。
实验方法结果
2.1太子参乙酸乙酯提取HPLC分析
称取太子参（粉碎过三号筛）200g，加入4L乙酸乙酯，90℃索氏提取4h。冷却至室温，旋转蒸发仪上减压回收溶剂至干，以色谱纯的甲醇溶解，0.22μm微孔滤膜过滤，供HPLC分析。
HPLC分析的色谱条件为：大连依利特Hypersil ODS色谱柱（4.6mm×250mm，5μm）；流速：1mL/min；进样量：20μL；柱温：30℃；检测波长：203nm；时间：90min；流动相：A：乙腈；B：0.2%磷酸水。梯度洗脱程序见表1，太子参乙酸乙酯提取物的HPLC指纹图谱见图1。
表1 流动相梯度洗脱程序
2.2石油醚脱脂
太子参乙酸乙酯提取物置于循环超声波提取机中，加入石油醚（药液比=1:20 g/mL），室温超声脱脂1h，抽滤，弃去石油醚液，滤渣连续石油醚脱脂3次。滤渣挥干溶剂，加入无水乙醇（药液比=1:20 g/mL），60℃超声提取1 h，抽滤，冷却至室温，提取液于旋转蒸发仪上减压回收乙醇至干。
萃取除氨基酸
所得残渣用50mL热水充分溶解后置于分液漏斗中，用乙酸乙酯萃取3次，每次乙酸乙酯用量为100mL，乙酸乙酯相浓缩至干后，继续加50mL热水充分溶解置分液漏斗，加入水饱和正丁醇萃取3次，每次水饱和正丁醇的用量为50mL，合并正丁醇相倒入分液漏斗，用150mL 40%氨试液充分振摇，萃取3次，弃去氨试液，正丁醇相浓缩至干；残渣继续加50mL热水充分溶解，用氯仿萃取3次，每次氯仿用量为50mL，最后将氯仿相减压浓缩至干。
醇沉除糖及其他杂质
残渣置于烧杯中，加适量无水乙醇溶解后，静置12h，抽滤，滤液即为澄清的醇溶液。
冻干
将上述2.4项下所得醇溶液置烧杯中，按体积比1:1加入蒸馏水混合，即得50vol%醇溶液（凝固点-25℃），置-80℃冰箱预冻后置于真空冷冻干燥机冷冻干燥，即得淡黄色粉末。
太子参环肽群验证
3.1 提取物冻干粉HPLC指纹图谱分析
取冻干粉末少许，加甲醇溶解，用0.22μm的微孔滤膜过滤，置于进样瓶中，作为供试品溶液。
HPLC色谱条件：大连依利特Hypersil ODS色谱柱（4.6mm×250mm，5μm）；流速：1mL/min；进样量：20μL；柱温：30℃；检测波长：203nm；时间：90min；流动相：A：乙腈；B：0.2%磷酸水。按表1梯度洗脱程序，色谱图见图2，峰面积信息见表2。
表2 峰面积信息表
HPLC色谱图可见，提取物冻干粉甲醇溶液中，峰面积在0.01%以上的组分40个。通过UHPLC-QTof/MS对太子参提取液进行分析，在ESI源正负离子模式下，共鉴定了峰面积大于1%的16个化合物（见表3），其中峰2~峰10、峰12~峰14均为环肽化合物，按归一化法计算，环肽分子群占总提取物的92.93%。
表3 16个成分信息表环肽类化合物名称
以上所述仅为本发明的较佳实施例，凡依本发明申请专利范围所做的均等变化与修饰，皆应属本发明的涵盖范围。
Claims (1)
1.一种太子参环肽提取物的制备方法，其特征在于：包括以下步骤：
1）提取：将太子参粉碎，过三号筛，按料液比1:20 g/mL加入乙酸乙酯，于90℃索氏提取4h，然后将提取液冷却至室温，旋蒸去除溶剂，得太子参乙酸乙酯提取物；
2）脱脂：将太子参乙酸乙酯提取物置于循环超声波提取机中，按料液比1:20 g/mL加入石油醚进行超声脱脂，然后抽滤，所得滤渣重复石油醚脱脂3次后，挥干溶剂，再按料液比1:20 g/mL加入无水乙醇，60℃超声提取1 h，然后抽滤，滤液冷却至室温后旋蒸去除溶剂；
3）除氨基酸：将步骤2）脱脂后的残渣用热水充分溶解后，按体积比1:2加入乙酸乙酯，萃取3次，所得乙酸乙酯萃取相浓缩至干后，重新溶解于热水中，再按体积比1:1加入水饱和正丁醇，萃取3次，所得正丁醇相按体积比1:1加入40 vol%的氨试液，萃取3次，然后弃去氨试液，收集正丁醇相浓缩至干，所得残渣继续溶解于热水中，再按体积比1:1加入氯仿，萃取3次，所得氯仿相减压浓缩至干；
4）醇沉：将步骤3）所得残渣加无水乙醇溶解后，静置12h，抽滤，收集滤液；
5）冻干：将步骤4）所得滤液加水配成50vol%醇溶液，于-80℃预冷冻后进行冷冻干燥，即得太子参环肽提取物；
所得太子参环肽提取物中总环肽含量在92%以上。
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