CN111603509A - 一种富含二氢杨梅素的枳椇子提取物制备方法 - Google Patents

一种富含二氢杨梅素的枳椇子提取物制备方法 Download PDF

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CN111603509A
CN111603509A CN202010616851.4A CN202010616851A CN111603509A CN 111603509 A CN111603509 A CN 111603509A CN 202010616851 A CN202010616851 A CN 202010616851A CN 111603509 A CN111603509 A CN 111603509A
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hovenia dulcis
dulcis thunb
dihydromyricetin
ethanol
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谷素静
文雁君
李林正
金子恒
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Henan Zhongda Hengyuan Biotechnology Stock Co Ltd
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Abstract

本发明提供一种富含二氢杨梅素的枳椇子提取物制备方法，包括枳椇子用乙醇水搅拌提取，提取液过滤分离，真空浓缩回收至一定固形物含量的浓缩液，浓缩液冷藏放置分层，将分层的浓缩液进行离心分离，取上清液喷雾干燥呈粉末，既得枳椇子提取物。枳椇子提取物二氢杨梅素含量高达10％以上。同时，产品水溶性良好，水溶液澄清透亮，与现存市场上枳椇子提取物相比，浊度低，且二氢杨梅素含量高，增加其在食品保健品等行业的实用性，扩大了适用范围。本发明方法多设备要求低，操作方便简单，可行，能够满足大规模工业化生产的需要。

Description

一种富含二氢杨梅素的枳椇子提取物制备方法
技术领域
本发明涉及药食同源原料，具体涉及有效成分的提取制备方法，尤其涉及一种富含二氢杨梅素的枳椇子提取物制备方法。
技术背景
枳椇子为鼠李科植物枳椇(Hovenia dulcis Thunb)的干燥成熟种子。现由《中华人民共和国卫生部药品标准.中药材》收载，即是食品又是药品的名单之一，具有清热，利尿，解酒毒之功效，主治酒病、烦热、口渴、呕吐、二便不利等症。枳椇子含有黄酮类活性成分山柰酚、洋芹素、杨梅黄素、槲皮素、氢杨梅黄素和蒽醌类化合物大黄素，其中二氢杨梅素的含量较高，且有极高的保肝活性，同时也具有抗炎、镇痛、降血脂、提高SOD活性，抑菌、抗病毒等药理功效。市场上对枳椇子提取物的要求已不仅限于黄酮含量，对二氢杨梅素含量也有要求。
目前，枳椇子提取工艺主要采用热水提取、低级醇提取或是酸碱提取，但是这些方法得到的提取物或是二氢杨梅素含量低、或是水中溶解状态差，很难满足饮料及口服液食品行业的要求。CN109601789A一种高澄清度水溶性的枳椇子提取物制备。该方法以黄酮为指标，用去离子水提取，趁热砂芯过滤，离心，再真空浓缩成固体粉碎而得的枳椇子提取物粉末。该方法采用水提总黄酮含量10％，回收率约60％，总黄酮收率及含量均较低，造成原料资源浪费，且采用真空浓缩粉碎干燥工艺能耗高，操作复杂。CN200810226063.3公开了一种枳椇子提取物及其制备方法与在制备抗肿瘤药物中的应用。该方法是用水和/或有机溶剂作为提取剂，从枳椇子中提取得到。所用有机溶剂为甲醇、乙醇、石油醚、氯仿、二氯甲烷、乙酸乙酯、正丁醇、苯或甲苯。该方法不仅使用了大量的有机溶剂，成本高，工艺复杂，而且得到的枳椇子提取物的水溶解性较差，水溶液浑浊，不能直接应用到食品饮料行业。
发明内容
为了克服背景技术所述的不足，本发明的目的在于解决枳椇子提取物在食品中溶解性的应用问题及品质提升的问题，提供一种水溶性良好富含二氢杨梅素的提取物的操作简便，低成本的制备方法。
本发明提供的一种富含二氢杨梅素的枳椇子提取物制备方法，包括下列步骤；
(1)原料处理：枳椇子原料，粉碎得枳椇子粉末；
(2)提取：加入药材总质量的3-15倍重量的10-95％乙醇溶液，于20℃-80℃搅拌提取；
(3)过滤：提取液过滤将料渣分离；
(4)减压浓缩：蒸发去除过滤液中的乙醇提取溶剂；将滤液减压浓缩至浸膏，浸膏固形物含量10％-40％；
(5)冷藏静置：将浸膏放置低温-20℃-8℃状态下静置分层；
(6)离心：将分层的浓缩液进行离心分离，得上清液，
(7)干燥：上清液喷雾干燥，得枳椇子提取物粉末。
本发明的一种富含二氢杨梅素的枳椇子提取物制备方法，其优选方案中，步骤(1)原料处理为：取干燥枳椇子，制成粗粉，过20目筛。
优选的，步骤(2)中，加入原料总重量的3-12倍重量的乙醇溶液，乙醇浓度为30-85％，提取温度20-70℃，搅拌提取1-4h，提取2次，合并提取液。
优选的步骤(2)中，加入原料总重量的6倍重量的乙醇溶液，乙醇浓度为70％，提取温度为60℃，搅拌提取1h,提取2次，合并提取液。
优选的，步骤(3)中，将提取液进行板框过滤。
优选的，所述步骤(4)中，采用旋转蒸发，去除过滤液中的乙醇提取溶剂，旋转蒸发的温度为60-80℃，真空度为-0.06-0.095Mpa；将滤液减压浓缩至浸膏，浸膏固形物含量10％-40％。
优选的，所述步骤(5)中，将浸膏放置-20℃-8℃，放置时间为0.5h-12小时。
优选的，所述步骤(6)中，将冷藏的浸膏进行离心，离心速率2000-5000r/min。
优选的，所述步骤(4)中，将滤液减压浓缩至浸膏，浸膏固形物含量为25％；所述步骤(5)中，将浸膏放置0℃，放静置3h；所述步骤(6)中，离心速率为3000r/min。
本发明提供一种富含二氢杨梅素的枳椇子提取物制备方法，包括枳椇子用乙醇水搅拌提取，提取液过滤分离，真空浓缩回收至一定固形物含量的浓缩液，浓缩液冷藏放置分层，将分层的浓缩液进行离心分离，取上清液喷雾干燥呈粉末，既得枳椇子提取物。枳椇子提取物二氢杨梅素含量高达10％以上。同时，产品水溶性良好，水溶液澄清透亮，与现存市场上枳椇子提取物相比，浊度低，且二氢杨梅素含量高，增加其在食品保健品等行业的实用性，扩大了适用范围。本发明方法多设备要求低，操作方便简单，可行，能够满足大规模工业化生产的需要。
具体实施方式
实施例1：
取枳椇子原料1kg，制成粗粉，过20目筛，加入70％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，合并提取液，板框过滤，减压回收乙醇，得固形物含量25％浸膏，再将浸膏至于0℃冷藏静置3h,3000r/min,离心10分钟，得离心液直接进行喷雾干燥，得94.8g枳椇子提取物，二氢杨梅素提取率82.6％，含量12.2％，2‰水溶液澄清透亮，浊度0.8NTU.,
实施例2：
取枳椇子原料1kg，制成粗粉，过20目筛，加入70％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，合并提取液，板框过滤，减压回收乙醇，得固形物含量45％浸膏，再将浸膏至于室温20℃静置3h,3000r/min,离心10分钟，得离心液直接进行喷雾干燥，得166g枳椇子提取物，二氢杨梅素提取率80.7％，含量6.8％，2‰水溶液大量沉淀物。
实施例3：
取枳椇子原料1kg，制成粗粉，过20目筛，加入30％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，合并提取液，板框过滤，减压回收乙醇，得固形物含量45％浸膏，再将浸膏至于0℃冷藏静置12h,3000r/min,离心10分钟，得离心液直接进行喷雾干燥，得163g枳椇子提取物，二氢杨梅素提取率67.6％，含量5.8％，2‰水溶液浑浊，浊度54NTU.,
对比例
取枳椇子原料1kg，制成粗粉，过20目筛，加入95％％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，合并提取液，板框过滤，减压回收乙醇，得浸膏，真空干燥至恒重，得123g枳椇子提取物，二氢杨梅素提取率24.2％，含量2.7％，2‰水溶液浑浊，有大量漂浮物及沉淀。
本发明与CN10390979专利产品对比结果见下表：
Figure BDA0002561975540000051
可见，本发明得到的枳椇子提取物在水中溶解性极佳，二氢杨梅素含量高，得率高，可用于食品饮料及口服液。工艺操作简单可行，适用于工业化生产。
最后应说明的是：显然，上述实施例仅仅是为清楚地说明本发明所作的举例，而并非对实施方式的限定。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。而由此所引伸出的显而易见的变化或变动仍处于本发明的保护范围之中。

Claims (10)

1.一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，该方法包括下列步骤；
(1)原料处理：枳椇子原料，粉碎得枳椇子粉末；
(2)提取：加入药材总质量的3-15倍重量的10-95％乙醇溶液，于20℃-80℃搅拌提取；
(3)过滤：提取液过滤将料渣分离；
(4)减压浓缩：蒸发去除过滤液中的乙醇提取溶剂；将滤液减压浓缩至浸膏，浸膏固形物含量10％-40％；
(5)冷藏静置：将浸膏放置低温-20℃-8℃状态下静置分层；
(6)离心：将分层的浓缩液进行离心分离，得上清液，
(7)干燥：上清液喷雾干燥，得枳椇子提取物粉末。
2.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，步骤(1)原料处理为：取干燥枳椇子，制成粗粉，过20目筛。
3.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，步骤(2)中，加入原料总重量的3-12倍重量的乙醇溶液，乙醇浓度为30-85％，提取温度20-70℃，搅拌提取1-4h，提取2次，合并提取液。
4.根据权利要求3所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，步骤(2)中，加入原料总重量的6倍重量的乙醇溶液，乙醇浓度为70％，提取温度为60℃，搅拌提取1h,提取2次，合并提取液。
5.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，步骤(3)中，将提取液进行板框过滤。
6.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，所述步骤(4)中，采用旋转蒸发，去除过滤液中的乙醇提取溶剂，旋转蒸发的温度为60-80℃，真空度为-0.06-0.095Mpa；将滤液减压浓缩至浸膏，浸膏固形物含量10％-40％。
7.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，所述步骤(5)中，将浸膏放置-20℃-8℃，放置时间为0.5h-12小时。
8.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，所述步骤(6)中，将冷藏的浸膏进行离心，离心速率2000-5000r/min。
9.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，所述步骤(4)中，将滤液减压浓缩至浸膏，浸膏固形物含量为25％；所述步骤(5)中，将浸膏放置0℃，放静置3h；所述步骤(6)中，离心速率为3000r/min。
10.根据权利要求1所述的一种富含二氢杨梅素的枳椇子提取物制备方法，其特征在于，包括如下步骤：取枳椇子原料1kg，制成粗粉，过20目筛，加入70％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，合并提取液，板框过滤，减压回收乙醇，得固形物含量25％浸膏，再将浸膏至于0℃冷藏静置3h,3000r/min,离心10分钟，得离心液直接进行喷雾干燥，得枳椇子提取物。
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