CN108785373B - 一种冬凌草超微粉及其制备方法 - Google Patents
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Abstract
本发明涉及中药技术领域，公开了一种冬凌草超微粉及其制备方法。本发明所述冬凌草包括冬凌草、β‑环糊精和A组分，所述A组分为淀粉或气相二氧化硅。本发明选择淀粉或气相二氧化硅作为辅助成分，联合β‑环糊精对冬凌草进行超微粉碎，借助超微粉碎的物理作用，将从冬凌草中释放出来的甲素等物质引入β‑环糊精立体筒状手性疏水空腔，起到保护作用，避免长时间放置导致的甲素含量明显下降的现象。
Description
技术领域
本发明涉及中药技术领域，特别涉及一种冬凌草超微粉及其制备方法。
背景技术
冬凌草Rabdosiarubescens(Hemsl.)Hara，又名冰凌草，为唇形科香茶菜属多年生草本植物，以地上部分入药，广泛分布于我国黄河长江流域，主产于河南济源太行山一带。味甘苦，性微寒，具有清热解毒、消炎止痛、健胃活血及抗肿瘤之功效。用于治疗咽喉肿痛、急性喉炎、急性化脓性扁桃体炎、慢性支气管炎及慢性咽炎、蛇虫咬伤，对食管癌、贲门癌、原发性肝癌、肺癌、乳癌、前列腺癌、膀胱癌等有明显缓解症状作用，有稳定和缩小瘤体及延长患者生命的效果。1977年，冬凌草被收入《中华人民共和国药典》，并编入《全国中草药汇编》。冬凌草抗癌功能出色，对多种肿瘤有效，同时与现有化疗药物配伍使用，不仅能大大提高后者的抑瘤效果，还可降低其用量及毒副作用。进入21世纪，有着“紫杉醇第二”之称的冬凌草已成为国内外肿瘤学者竞相研究的热点。(冯卫生，李红伟，郑晓珂，王彦志冬凌草化学成分研究进展《中国新药杂志》2008年,17卷,28期)
正是因为冬凌草具有广谱的杀菌、抑菌、消炎、良好的生物学活性且低毒性、抗肿瘤防癌等功效，多年来国内对冬凌草的有效成分提取及应用十分活跃，同时也引起了国外对冬凌草的研究及应用的重视。
传统的冬凌草复合有效物和单品成分的提取一般都是采用煎煮、乙醇浸提、微波提取、超临界萃取、溶剂萃取--大孔离子交换提取等方法。冬凌草中的主要有效物例如甲素、乙素在提取过程中，容易受高温、时间、高能微波的影响而降解。而且，近年来采用蒸煮--乙醇浸取--浓缩--加工成冬凌草片剂、膏剂、丸剂等，产品在仓储存放期、市场货架期、销售流动期中，其中有效活性物例如甲素，很容易降解，严重的影响了产品的质量。于是，做为中药冬凌草系列产品的开发，其有效活性物的温和的提取方法是保证下游产品开发的很重要的一环。
超微粉碎是近年来发展非常迅速的一项新技术。应用这种技术，可将固体物质粉碎成直径小于10μm的超微粉体，因而，经超微粉碎处理的粉体具有良好的溶解性、分散性、吸附性及化学反应活性。超微粉碎的细胞破壁率可达90％以上。所以，将它应用于中药制剂的生产过程中，可大幅度提高药材中有效成分在体内的释放和吸收，提高中药制剂的药效。
但是，冬凌草超微粉在经过长时间放置后，依然会存在甲素等活性物质含量铭明显下降的现象，因此需要对冬凌草超微工艺进行改进，避免甲素活性物质含量明显下降的现象。
发明内容
有鉴于此，本发明的目的在于提供一种冬凌草超微粉及其制备方法，使得所述冬凌草超微粉在长时间储存后依旧保持高含量甲素。
为实现上述发明目的，本发明提供如下技术方案：
一种冬凌草超微粉，包括冬凌草、β-环糊精和A组分，所述A组分为淀粉或气相二氧化硅。
针对冬凌草超微粉长时间放置导致活性物质甲素含量明显下降的缺陷，本发明在冬凌草基础上增加了β-环糊精，以及淀粉或气相二氧化硅一同进行超微粉碎，解决了上述问题。
在本发明具体实施方式中，所述冬凌草、β-环糊精和A组分的质量比为1:0.5:0.5。
β-环糊精是由7个葡萄糖分子以1,4糖苷键连接而成，主体构像是一个中间有空洞，两端不封闭的圆筒，其显著的结构特征是存在一个立体筒状手性疏水空腔，特殊的非极性疏水环境使β-环糊精能以范德华力、疏水和氢键等作用力，与一些极性、大小、形状及性质相匹配的分子或某些分子的疏水性基团作用，在其空间结构中全部或部分包入另一种分子形成稳定的超分子包合化合物。然而，β-环糊精在对目标物质包合过程中普遍需要在水溶液环境中，而直接以固体形式进行，并不会有很好的包合效果。
为此，本发明特别选择了淀粉或气相二氧化硅作为辅助物质，在超微粉碎过程中，冬凌草被粉碎成超细粒子，由于破壁效果，冬凌草单萜、二萜、三萜等萜类化合物如甲素、乙素、齐墩果酸、熊果酸等得以释放出来，在β-环糊精，以及淀粉或气相二氧化硅作用下，进入β-环糊精立体筒状手性疏水空腔，因此对这些物质起到一定的保护作用。
在本发明对比试验中，以冬凌草和冬凌草+β-环糊精作为两种对照组进行超微粉碎，在经过长达240天的放置后，检测各自甲素的含量，结果显示，本发明冬凌草超微粉甲素含量的损失百分比均未超过1.5％，而对照组的甲素含量损失百分比达到了7-20％。由此表明，本发明冬凌草超微粉具备更高的稳定性，可避免甲素含量的显著下降。
此外，本发明还提供了所述超微粉的制备方法，包括：
步骤1、将冬凌草杀菌和清洗；
步骤2、无菌条件下，干燥冬凌草，然后将冬凌草、β-环糊精和A组分在不锈钢普通粉碎机上粉碎成粗粉；
步骤3、然后将所述粗粉进行超微粉碎，获得所述超微粉。
作为优选，步骤1为：
步骤1.1、将冬凌草在置紫外灯的震动传送网上进行照射消毒杀菌，以消除附着叶片上的虫卵细菌以及抖落叶片上的灰尘；
步骤1.2、将紫外处理过的冬凌草叶片加到恒温25℃矿化活化水中清洗。
作为优选，步骤2中所述干燥冬凌草为真空干燥冬凌草至其含水量＜1％，所述真空干燥的真空度在0.05-0.085mpa，温度在25-35℃；步骤2中所述不锈钢普通粉碎机为不锈钢普通链锤式粉碎机；步骤2中所述粗粉粒度＜100目。
作为优选，步骤3为：
将所述粗粉装入真空高能研磨超微粉碎机、封闭式链锤切割式高能磨超微粉碎机或重压研磨式超微粉碎机上超微粉碎4h，获得所述超微粉。
由以上技术方案可知，本发明选择淀粉或气相二氧化硅作为辅助成分，联合β-环糊精对冬凌草进行超微粉碎，借助超微粉碎的物理作用，将从冬凌草中释放出来的甲素等物质引入β-环糊精立体筒状手性疏水空腔，起到保护作用，避免长时间放置导致的甲素含量明显下降的现象。
具体实施方式
本发明公开了一种冬凌草超微粉及其制备方法，本领域技术人员可以借鉴本文内容，适当改进工艺参数实现。特别需要指出的是，所有类似的替换和改动对本领域技术人员来说是显而易见的，它们都被视为包括在本发明。本发明所述超微粉及其制备方法已经通过实施例进行了描述，相关人员明显能在不脱离本发明内容、精神和范围内对本文所述超微粉及其制备方法进行改动或适当变更与组合，来实现和应用本发明技术。
在本发明具体实施例中，涉及到对比试验，各试验组除了应有的区别外，其余试验环境和原材料等均保持一致。
以下就本发明所提供的一种冬凌草超微粉及其制备方法做进一步说明。
实施例1：制备本发明冬凌草超微粉
将采摘晒干的冬凌草全草在置紫外灯的震动传送网上进行照射、消毒、杀菌，以消除附着叶片上的虫卵细菌以及抖落叶片上的灰尘；
将紫外处理过的冬凌草全草加入到恒温25℃矿化活化水中迅速清洗，清洗方式最好为快速浸取，浸取时间为2--5分钟。
以下的工序环境要求为超净无菌环境：
将浸取的冬凌草全草沥干大量的水分立即进行离心甩干；甩干的冬凌草全草在真空干燥条件下烘干至含水量＜1％，真空度在0.07mpa，温度在28℃；
将冬凌草、β-环糊精和A组分按照1:0.5:0.5的质量比，在不锈钢普通链锤式粉碎机上粉碎成粒度＜100的粗粉；然后再在真空高能研磨超微粉碎机粉碎时间4小时，真空度为0.09MPa，粉碎所得超微粉即为所述冬凌草超微粉；
检测所述冬凌草超微粉以及对照组(按照上述工艺仅采用冬凌草以及冬凌草+β-环糊精进行制备，用量保持一致)的甲素含量，连续跟踪240天，观察经过超微粉碎后冬凌草主成分甲素的含量变化，结果见表1。
表1
由表1可知，对照组甲素含量损失的百分比分别为7.9％和9.2％，而本发明两组超微粉冬凌草甲素含量损失的百分比均仅为1.3％。
实施例2：制备本发明冬凌草超微粉
将采摘晒干的冬凌草全草在置紫外灯的震动传送网上进行照射、消毒、杀菌，以消除附着叶片上的虫卵细菌以及抖落叶片上的灰尘；
将紫外处理过的冬凌草全草加入到恒温25℃矿化活化水中迅速清洗，清洗方式最好为快速浸取，浸取时间为2--5分钟。
以下的工序环境要求为超净无菌环境：
将浸取的冬凌草全草沥干大量的水分立即进行离心甩干；甩干的冬凌草全草在真空干燥条件下烘干至含水量＜1％，真空度在0.07mpa，温度在28℃；
将冬凌草、β-环糊精和A组分按照1:0.5:0.5的质量比，在不锈钢普通链锤式粉碎机上粉碎成粒度＜100的粗粉；然后再在封闭式链锤切割式高能磨超微粉碎机粉碎时间4小时，粉碎所得超微粉即为所述冬凌草超微粉；
检测所述冬凌草超微粉以及对照组(按照上述工艺仅采用冬凌草以及冬凌草+β-环糊精进行制备，用量保持一致)的甲素含量，连续跟踪240天，观察经过超微粉碎后冬凌草主成分甲素的含量变化，结果见表2。
表2
由表2可知，对照组甲素含量损失的百分比均为10.5％，而本发明冬凌草甲素含量损失的百分比均仅为1.3％。
实施例3：制备本发明冬凌草超微粉
将采摘晒干的冬凌草全草在置紫外灯的震动传送网上进行照射、消毒、杀菌，以消除附着叶片上的虫卵细菌以及抖落叶片上的灰尘；
将紫外处理过的冬凌草全草加入到恒温25℃矿化活化水中迅速清洗，清洗方式最好为快速浸取，浸取时间为2--5分钟。
以下的工序环境要求为超净无菌环境：
将浸取的冬凌草全草沥干大量的水分立即进行离心甩干；甩干的冬凌草全草在真空干燥条件下烘干至含水量＜1％，真空度在0.07mpa，温度在28℃；
将冬凌草、β-环糊精和A组分按照1:0.5:0.5的质量比，在不锈钢普通链锤式粉碎机上粉碎成粒度＜100的粗粉；然后再在重压研磨式超微粉碎机粉碎时间4小时，粉碎所得超微粉即为所述冬凌草超微粉；
检测所述冬凌草超微粉以及对照组(按照上述工艺仅采用冬凌草以及冬凌草+β-环糊精进行制备，用量保持一致)的甲素含量，连续跟踪240天，观察经过超微粉碎后冬凌草主成分甲素的含量变化，结果见表3。
表3
由表3可知，对照组甲素含量损失的百分比分别为9.375％和8.3％，而本发明冬凌草甲素含量损失的百分比仅为1.1％。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (4)
1.一种冬凌草超微粉，其特征在于，由冬凌草、β-环糊精和A组分组成，所述A组分为淀粉或气相二氧化硅；所述冬凌草、β-环糊精和A组分的质量比为1:0.5:0.5；所述冬凌草超微粉在冬凌草基础上增加了β-环糊精，以及淀粉或气相二氧化硅一同进行超微粉碎；
所述超微粉的制备方法，包括：步骤1、将冬凌草杀菌和清洗；步骤2、无菌条件下，干燥冬凌草，干燥冬凌草为真空干燥冬凌草至其含水量＜1％，真空度在0.05-0.085mpa，温度在25-35℃；然后将冬凌草、β-环糊精和A组分在不锈钢普通粉碎机上粉碎成粗粉，粗粉粒度＜100目；步骤3、然后将所述粗粉进行超微粉碎，获得所述超微粉。
2.根据权利要求1所述冬凌草超微粉，其特征在于，步骤1为：步骤1.1、将冬凌草在置紫外灯的震动传送网上进行照射消毒杀菌，以消除附着叶片上的虫卵细菌以及抖落叶片上的灰尘；
步骤1.2、将紫外处理过的冬凌草叶片加到恒温25℃矿化活化水中清洗。
3.根据权利要求1所述冬凌草超微粉，其特征在于，步骤2中所述不锈钢普通粉碎机为不锈钢普通链锤式粉碎机。
4.根据权利要求1所述冬凌草超微粉，其特征在于，步骤3为：将所述粗粉装入真空高能研磨超微粉碎机、封闭式链锤切割式高能磨超微粉碎机或重压研磨式超微粉碎机上超微粉碎4h，获得所述超微粉。
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