CN114181051B - 一种桃柁酚的制备方法及其应用 - Google Patents
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Abstract
本发明公开了一种桃柁酚的制备方法及其应用，以柏树为原料，包括原材料前处理和改进的提取工艺，提取结合超临界二氧化碳萃取、溶剂萃取和超滤膜提纯，有效提升产物纯度。采用柏树为原料，拓宽了原料来源，解除了原料的地域限制，使产物可有效全面推广，通过改进的提取工艺提取得到纯度更好的桃柁酚，且工艺简便易操作，适合大量生产。
Description
技术领域
本发明涉及化合物的提取和应用技术领域，更具体的说是涉及一种桃柁酚的制备方法及其应用。
背景技术
桃柁酚(TOTAROL)是一种芳香族二萜化合物，是从Totara(桃拓罗汉松)树的心材中提取的天然物质。桃柁酚有广谱的抗菌特性，有效对抗金黄色酿脓葡萄球菌(包括耐甲氧西林、传染菌群落、多重耐药菌株等)，变形链球菌、耐青霉素的肺炎链球菌、耐红霉素的链球菌、耐庆大霉素的粪肠球菌、耐阴肠球菌、门斯顿沙门氏菌、大肠杆菌、产气肠杆菌、铜绿假单胞菌、枯草芽孢杆菌、氨短杆菌和痘丙酸杆菌等。桃拓酚的其他特性令它具有更多潜在的用途。例如，Totarol的贝塔-氨基醇衍生物已证明具有抗疟原虫特性，且与氯喹无交叉耐药，对结核分歧杆菌有活性。
Totarol拥有的一系列生物活性及相关技术，使其成为多种应用领域的关键抗炎剂，包括:化妆品、伤口护理、口腔护理品、个人护理品/补充剂、药品、动物护理品等方面，但是现有的桃柁酚均是采用生长于新西兰的桃拓罗汉松的枯木进行提取，限制了其地域性，现有研究发现，在其它植物(例如：柏树、杜松、金钟柏、迷迭香等)体中也具有桃柁酚成分，但是现有技术中缺乏从其它植物中提取桃柁酚的技术，其本身限制了桃柁酚的广泛应用。
因此，如何提供一种适用于其它植物中桃柁酚的提取技术是本领域技术人员亟待解决的问题。
发明内容
有鉴于此，本发明提供了一种桃柁酚的制备方法，采用来源广泛的柏树为原料，通过改进工艺进行提取制备桃柁酚。
为实现上述目的，本发明采用如下技术方案：
一种桃柁酚的制备方法，以柏树为原料，包括以下步骤：
步骤一：原料处理
取柏树枯木进行粉碎，之后将粉碎后的木屑采用红外冲击干燥，备用；
步骤二：有效组分的提取
(2.1)对步骤一中干燥后的木屑进行研磨，然后采用超临界二氧化碳提取；
(2.2)提取后物质采用溶剂萃取，超滤膜过滤后，收集截留物，蒸发溶剂得到桃柁酚。
优选的，步骤一种所述的红外冲击干燥采用安装有近红外辐射器的干燥箱，近红外辐射器与样品距离300mm，散热器在全功率下产生1.2μm，2100℃的峰值辐射。
优选的，步骤一中所述的干燥至含水率≤15％。
优选的，步骤(2.1)中所述的研磨至粒径≤3mm。
优选的，步骤(2.1)中所述的超临界二氧化碳提取温度为45-55℃、压力为300bar，二氧化碳流体流量4000kg/h，超临界二氧化碳萃取的周期为3h。
优选的，步骤(2.2)中所述的萃取溶剂为乙醇或丁二醇。
优选的，步骤(2.2)中所述的超滤膜截留分子量为286.5道尔顿。
本发明还提供了一种如上技术方案中方法制得的桃柁酚的应用，即应用于抑菌制品的制备，抑菌制品包括但不限于女性私护抑菌等。
优选的，所述的桃拓酚在抑菌产品中添加量为产品总质量的0.01％-1％。
经由上述的技术方案可知，与现有技术相比，本发明公开提供了一种桃柁酚的制备方法和应用，具有如下有益效果：
采用柏树为原料，拓宽了原料来源，解除了原料的地域限制，使产物可有效全面推广，通过改进的提取工艺提取得到纯度更好的桃柁酚，且工艺简便易操作，适合大量生产。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据提供的附图获得其他的附图。
图1为本发明实施例1制备的桃柁酚对金黄色葡萄球菌的作用扫描电镜图；
图2为本发明实施例1制备的桃柁酚对金黄色葡萄球菌的作用透视电镜图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，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
桃柁酚的制备方法，以柏树为原料，包括以下步骤：
步骤一：原料处理
取柏树枯木进行粉碎，之后将粉碎后的木屑采用红外冲击干燥，红外冲击干燥采用安装有近红外辐射器的干燥箱，近红外辐射器与样品距离300mm，散热器在全功率下产生1.2μm，2100℃的峰值辐射，干燥至含水率≤15％备用；
步骤二：有效组分的提取
(2.1)对步骤一中干燥后的木屑进行研磨至粒径≤3mm，然后采用超临界二氧化碳提取，超临界二氧化碳提取温度为45-55℃、压力为300bar，二氧化碳流体流量4000kg/h，超临界二氧化碳萃取的周期为3h；
(2.2)提取后物质采用乙醇萃取，之后以截留分子量为286.5道尔顿超滤膜过滤后，收集截留物，蒸发溶剂得到桃柁酚。
试验例
1)对实施例1制得的桃拓酚进行检测，结果如下表所示：
| 产品名称 | 桃柁酚 |
| 项目 | 指标 |
| 外观 | 浅黄色至浅棕色澄清液体 |
| 干重含量 | ≥1％ |
| 重金属 | 未检出 |
| 砷 | 未检出 |
| 微生物总数 | 未检出 |
| 大肠杆菌 | 未检出 |
| 沙门氏菌 | 未检出 |
检测结果表明，本发明方法制得的桃拓酚纯度合格且符合各项指标。
2)采用实施例1制得的产物，溶解于乙醇中，制成质量百分比1％的提取液，之后将该提取液添加至含有金黄色葡萄球菌的培养基中，添加量为培养基总重量的0.05％，分别记录初始状态培养基、添加1h、1.5h、2h、2.5h、3h后的培养基的扫描电镜图和透视电镜图，结果如附图1-2所示，附图1-2中的a-f分别对应初始状态培养基、添加1h、1.5h、2h、2.5h、3h后的培养基的扫描电镜图和透视电镜图，附图1-2显示，金黄色葡萄球菌菌体细胞经过桃柁酚的作用处理后，受到了严重的损伤，并且，随着桃柁酚作用菌体细胞的时间不断延长，菌体受损的情况也不断加重。由图可得知桃柁酚破坏了细菌细胞膜的完整性，具有良好的抑菌作用。
3)抑菌效果检测
上述检测结果表明，本发明的技术方案制得的桃拓酚具有良好的抑菌作用。
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言，由于其与实施例公开的方法相对应，所以描述的比较简单，相关之处参见方法部分说明即可。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (4)
1.一种桃柁酚提取物的制备方法，其特征在于，以柏树为原料，包括以下步骤：
步骤一：原料处理取柏树枯木进行粉碎，之后将粉碎后的木屑采用红外冲击干燥，备用；
步骤二：有效组分的提取
(2.1)对步骤一中干燥后的木屑进行研磨，然后采用超临界二氧化碳提取；
(2.2)提取后物质采用溶剂萃取，超滤膜过滤后，收集截留物，蒸发溶剂得到桃柁酚；
步骤一中所述的红外冲击干燥时近红外辐射器与样品距离300mm，散热器在全功率下产生1.2μm，2100℃的峰值辐射；干燥至含水率≤15％；
步骤(2.1)中所述的研磨至粒径≤3mm；所述的超临界二氧化碳提取温度为45-55℃、压力为300bar，二氧化碳流体流量4000kg/h，超临界二氧化碳萃取的周期为3h；
步骤(2.2)中所述的萃取溶剂为乙醇或丁二醇；所述的超滤膜截留分子量为286.5道尔顿。
2.根据权利要求1所述的一种桃柁酚提取物的制备方法，其特征在于，步骤一中所述的红外冲击干燥采用安装有近红外辐射器的干燥箱进行干燥。
3.一种权利要求1或2的方法制得的桃柁酚提取物在抑菌制品中的应用。
4.根据权利要求3所述的一种桃柁酚提取物的应用，其特征在于，所述桃柁酚提取物的添加量为0.01wt％-1wt％。
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| KR20120019551A (ko) * | 2010-08-26 | 2012-03-07 | 신라대학교 산학협력단 | 소나무로부터 항균 활성 및 항산화 활성을 가진 물질을 생산하는 방법 |
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