CN103611333A - 固态酶解-co2流体超临界萃取蜂胶超级天然因子的方法 - Google Patents
固态酶解-co2流体超临界萃取蜂胶超级天然因子的方法 Download PDFInfo
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Abstract
本发明提供了一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，属于蜂胶提取加工技术领域。包括以下步骤：⑴原料预处理：选用优质毛胶为原料，经去杂、冷冻、粉碎；⑵原料固态酶解：加入酶解剂，均质混合后充填在固态酶解床上，通过调节酶解温度、湿度、pH、时间等参数进行固态酶解；⑶CO2流体超临界萃取。本发明的方法制得蜂胶超级天然因子成分全，特别是杨梅黄酮、槲皮素、芹菜素、松属素等黄酮苷元的含量得到提高，增强了蜂胶提取物的抗氧化活性，可更好地将蜂胶应用于医药、保健食品、化妆品等领域。
Description
技术领域
本发明涉及一种蜂胶中有效成分的萃取方法，特别涉及一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法,属于蜂胶提取加工技术领域。
背景技术
蜂胶（propolis）是由蜂群中的工蜂将采自杨树、柳树、松树等植物的幼芽和愈伤组织分泌的树脂状物质与自身的消化腺和蜡腺等腺体分泌物（如蜂蜡及多种消化酶）混合之后形成的一种黏性胶状物。蜂胶成分十分复杂，现已分离并鉴定出来的物质达300多种，其中黄酮类、萜烯类、脂肪族类和芳香族酸及其酯类化合物对人体有着明显的保健功能，如抗菌、消炎、抗病毒、降血糖血脂、增强免疫调节和抗肿瘤作用等。
近来,将超临界CO2流体萃取的技术应用于蜂胶提取中，特别是对蜂胶中的一些高附价值、热敏感性强、芳香性萜稀类物质、亲脂性分子量较小物质的萃取具有独特的效果。用超临界CO2流体萃取的技术萃取得到的蜂胶具有色泽淡黄、无溶剂残留、安全健康、杂质少、重金属含量低等优点。但超临界CO2流体萃取蜂胶技术存在一些技术难题：如物料的板结、勾流；对一些分子量太大的如苷类、多糖类等物质的分离萃取不彻底，从而导致萃取有效成分不全，萃取得率偏低等，这些问题制约了超临界萃取技术在蜂胶有效成分提取中的推广应 用，如何突破这些问题是本发明研究的方向。
固态酶解-CO2流体超临界萃取蜂胶超级天然因子技术就是将蜂胶原料先进行固态酶解，然后采用CO2流体超临界萃取技术萃取蜂胶超级天然因子。其基础学科依据是利用酶反应的高度专一性，通过酶的作用，对蜂胶中某些难以被CO2流体萃取的极性大，分子链长的物质进行分子结构的降解，变成极性小或短链小分子物质，如把蜂胶中的苷类、多糖类物质通过固态酶解技术降解成为糖苷元类物质，使其有效成分游离、混悬或胶溶于溶质中，再采用CO2流体超临界萃取技术萃取蜂胶超级天然因子，从而达到提高其萃取效率的目的。
发明内容
本发明所要解决的技术问题是固态酶解-CO2流体超临界萃取蜂胶超级天然因子，目的在于进一步提高超临界CO2流体萃取技术水平，提高萃取得率，降低生产成本，以便超临界CO2流体萃取技术在蜂胶提取中得到推广应用。该方法工艺简单，操作方便，无有机溶剂，极大的提高了生产效率且可大大提高黄酮类化合物的萃取含量。
为解决上述技术问题，本发明的技术方案是：
一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其特征在于，其制备方法如下：
1、毛胶的预处理：毛胶经预选分级，去除杂质。放入冷藏柜，置于-18℃温度下冷冻48h，冷冻后的毛胶，迅速放入破碎机中破碎或采用液氮冷冻的方式进行破碎，破碎成10-20目的颗粒，破碎后的原料，立即进入20目的震动筛，大于20目的颗粒返回冷藏柜;；
2、固态酶解：将破碎筛分后的毛胶配用水及复合酶系混合，后将混合原料铺在固态酶解床上，调节好相应的温湿度、PH值，进行固态酶解反应；
3、CO2流体超临界萃取：将经过固态酶解的蜂胶颗粒充填在萃取釜中，注入CO2流体进行萃取，萃取完毕后，系统压力降为常压，被萃取物析出，得蜂胶超级天然因子。
上述一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其中，所述的固态酶解反应酶选用β-鼠李糖苷酶、其酶用量为50-100IU/mg，β-葡萄糖苷酶、其酶用量为50-100IU/mg，木聚糖酶、其酶用量为1000-2000IU/mg，果胶酶、其酶用量为20-50IU/mg，α-淀粉酶、其酶用量为10-50IU/mg或复合酶系，加酶总量按重量百分比计为0.5-1.5％、酶解温度50-60℃、酶解湿度30-50%，酶解pH3.5-5.0，酶解时间12-24h。
上述一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其中，所述的CO2流体超临界萃取的工艺条件如下：萃取压力25-35MPa，萃取温度30-37℃，萃取时间150-240分钟，分离器压力6-10MPa，分离器温度40-55℃，二氧化碳流量为200-400L/H。
本发明的有益效果为：提高超临界CO2流体萃取技术水平，提高萃取得率，降低生产成本，以便超临界CO2流体萃取技术在蜂胶提取中得到推广应用。本方法工艺简单，操作方便，无有机溶剂，极大的提高了生产效率且可大大提高黄酮类化合物的萃取含量，本方法制得蜂胶超级天然因子成分全，特别是杨梅黄酮、槲皮素、芹菜素、松属素等黄酮苷元的含量得到提高，增强了蜂胶提取物的抗氧化活性， 可更好地将蜂胶应用于医药、保健食品、化妆品等领域。
附图说明
图1为经预处理后的毛胶（样品1）的总离子流色谱图
图2为经实例一得到的蜂胶超级天然因子（样品2）的总离子流色谱图
图3为经实例二得到的蜂胶超级天然因子（样品3）的总离子流色谱图
具体实施方式
以下通过具体实施例对本发明的具体实施方式作进一步详细的说明。
实例一
一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子，包括以下工艺步骤：
1、称取已去除杂质的毛胶150kg，置于-18℃温度下冷冻48h，采用液氮冷冻粉碎成10目的细颗粒（样品1）。
2、按毛胶原料重量比1:1加入复合酶系后将混合原料铺在生物酶解床上进行固态酶解反应，酶解温度50℃、酶解湿度35%，酶解pH4.0，酶解时间12h；其中，复合酶系由β-鼠李糖苷酶（酶用量50IU/mg）、β-葡萄糖苷酶（酶用量50IU/mg）、木聚糖酶（酶用量1000IU/mg）、果胶酶（酶用量20IU/mg）和α-淀粉酶（酶用量10IU/mg）组成。
3、将酶解完后的物料充填在萃取釜中，注入CO2流体萃取，萃取压力31MPa，萃取温度33℃，萃取时间240分钟，分离器压力8MPa，分离器温度48℃，二氧化碳流量为400L/H，萃取完毕后，系统压力降为常压，被萃取物析出，得蜂胶超级天然因子（样品2）。
实例二
一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子，包括以下工艺步骤：
1、称取已去除杂质的毛胶150kg，置于-18℃温度下冷冻48h，采用液氮冷冻粉碎成10目的细颗粒。
2、按毛胶原料重量比1:1加入复合酶系后将混合原料铺在生物酶解床上进行生物酶解反应，酶解温度60℃、酶解湿度50%，酶解pH5.5，酶解时间24h；其中，复合酶系由β-鼠李糖苷酶（酶用量100IU/mg）、β-葡萄糖苷酶（酶用量100IU/mg）、木聚糖酶（酶用量1000IU/mg）、果胶酶（酶用量50IU/mg）和α-淀粉酶（酶用量50IU/mg）组成。
3、将酶解完后的物料充填在萃取釜中，注入CO2流体萃取，萃取压力33MPa，萃取温度30℃，萃取时间240分钟，分离器压力6MPa，分离器温度45℃，二氧化碳流量为300L/H，萃取完毕后，系统压力降为常压，被萃取物析出，得蜂胶超级天然因子（样品3）
成分分析：
利用GC-MS法对采用固态酶解-CO2流体超临界萃取技术所得蜂胶超级天然因子进行成分分析。（样品1原料，样品2、样品3）
成分表：
从以上数据分析可以看出，蜂胶原料经固态酶解后再经CO2超临界萃取所得的蜂胶超级天然因子的成分较全。共鉴定出来85种化合物，其中79个定性，6个未检出，检出含量占总成分的96.46%。烯类有22种，共占总成分的42.32%，其中较多的AR－姜黄烯10.25%，姜黄烯6.22%，β－蛇床烯5.48%，α－蛇床烯2.31%，法尼烯2.93%，γ－杜松烯2.75%，β－愈创木烯1.68%；醇类有19种，共占总成分的24.41%，其中较多的苯甲醇4.9%，苯乙醇3.39%，β－桉叶醇1.37%，α－桉叶醇1.36%，愈创醇1.37%；酸类有8种，共占总成分的13.68%，其中较多的苯甲酸4.6%，2－甲基－2－丁烯酸4.29%，乙酸2.66%；醛类有8种，共占总成分的6.4%，其中较多的苯甲醛1.93%，肉桂醛1.23%；酯类有7种，共占总成分的2.37%；另外，醚、烷、酮、酚 类等相对含量共占总成分的7.28%。
这里本发明的描述和应用是说明性的，并非想将本发明的范围限制在上述实施例中，因此，本发明不受本实施例的限制，任何采用等效替换取得的技术方案均在本发明保护的范围内。
Claims (3)
1.一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其特征在于，其制备方法如下：
（1）、毛胶的预处理：毛胶经预选分级，去除杂质；
放入冷藏柜，置于-18℃温度下冷冻48h，冷冻后的毛胶，迅速放入破碎机中破碎或采用液氮冷冻的方式进行破碎，破碎成10-20目的颗粒，破碎后的原料，立即进入20目的震动筛，大于20目的颗粒返回冷藏柜；
（2）、固态酶解：将破碎筛分后的毛胶配用水及复合酶系混合，后将混合原料铺在固态酶解床上，调节好相应的温湿度、PH值，进行固态酶解反应；
（3）、CO2流体超临界萃取：将经过固态酶解的蜂胶颗粒充填在萃取釜中，注入CO2流体进行萃取，萃取完毕后，系统压力降为常压，被萃取物析出，得蜂胶超级天然因子。
2.如权利要求1所述的一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其特征为，所述的固态酶解反应酶选用β-鼠李糖苷酶、其酶用量为50-100IU/mg，β-葡萄糖苷酶、其酶用量为50-100IU/mg，木聚糖酶、其酶用量为1000-2000IU/mg，果胶酶、其酶用量为20-50IU/mg，α-淀粉酶、其酶用量为10-50IU/mg或复合酶系，加酶总量按重量百分比计为0．5-1.5％、酶解温度50-60℃、酶解湿度30-50%，酶解pH 3.5-5.0，酶解时间12-24h。
3.如权利要求1所述的一种固态酶解-CO2流体超临界萃取蜂胶超级天然因子的方法，其特征为，所述的CO2流体超临界萃取的工艺条件如下：萃取压力 25-35MPa，萃取温度30-37℃，萃取时间150-240分钟，分离器压力 6-10MPa，分离器温度40-55℃，二氧化碳流量为200-400L/H。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114028429A (zh) * | 2021-11-22 | 2022-02-11 | 江苏鸿祺生物科技有限公司 | 一种蜂胶活性组分超临界萃取原料的处理工艺 |
| CN114307235A (zh) * | 2021-12-10 | 2022-04-12 | 江苏鸿祺生物科技有限公司 | 一种高含量黄酮的蜂胶及其超临界萃取工艺 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5529779A (en) * | 1991-08-27 | 1996-06-25 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Purified propolis-extract, and its preparation and uses |
| CN101307344A (zh) * | 2008-07-08 | 2008-11-19 | 浙江大学 | 一种柚苷酶水解蜂胶黄酮苷的方法 |
| CN101530178A (zh) * | 2009-04-16 | 2009-09-16 | 江苏江大源生态生物科技有限公司 | 模拟生物流化床式超临界co2流体萃取蜂胶方法 |
| CN102321699A (zh) * | 2011-06-24 | 2012-01-18 | 江苏江大源生态生物科技有限公司 | 复合酶解辅助提取蜂胶中有效成份的方法 |
| CN102370667A (zh) * | 2011-10-26 | 2012-03-14 | 江苏江大源生态生物科技有限公司 | 一种超临界co2分离蜂胶中蜂蜡的方法 |
-
2013
- 2013-11-21 CN CN201310593710.5A patent/CN103611333A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5529779A (en) * | 1991-08-27 | 1996-06-25 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Purified propolis-extract, and its preparation and uses |
| CN101307344A (zh) * | 2008-07-08 | 2008-11-19 | 浙江大学 | 一种柚苷酶水解蜂胶黄酮苷的方法 |
| CN101530178A (zh) * | 2009-04-16 | 2009-09-16 | 江苏江大源生态生物科技有限公司 | 模拟生物流化床式超临界co2流体萃取蜂胶方法 |
| CN102321699A (zh) * | 2011-06-24 | 2012-01-18 | 江苏江大源生态生物科技有限公司 | 复合酶解辅助提取蜂胶中有效成份的方法 |
| CN102370667A (zh) * | 2011-10-26 | 2012-03-14 | 江苏江大源生态生物科技有限公司 | 一种超临界co2分离蜂胶中蜂蜡的方法 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114028429A (zh) * | 2021-11-22 | 2022-02-11 | 江苏鸿祺生物科技有限公司 | 一种蜂胶活性组分超临界萃取原料的处理工艺 |
| CN114028429B (zh) * | 2021-11-22 | 2022-12-16 | 江苏鸿祺生物科技有限公司 | 一种蜂胶活性组分超临界萃取原料的处理工艺 |
| CN114307235A (zh) * | 2021-12-10 | 2022-04-12 | 江苏鸿祺生物科技有限公司 | 一种高含量黄酮的蜂胶及其超临界萃取工艺 |
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