CN114984110A - 一种沉香提取工艺 - Google Patents
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Abstract
本发明公开一种沉香提取工艺，本方法将沉香样品过80目筛，以0.01g/mL(m:v)的浓度在体积浓度40％的乙醇—三氯甲烷溶液冷浸24h后，沉香浸提物总含量达225.21g/kg，浸提物总含量比方法一提高2.78倍，沉香四醇、2‑(2‑苯乙基)色酮、2‑(2‑(4‑甲氧基)苯乙基)色酮含量相较其他三种方法均达到了最高值，且该方法对沉香试样量要求低，在最大程度保留了沉香原有化学成分的同时，以经济、简便的方法显著提高了沉香浸提物含量。
Description
技术领域
本发明涉及沉香提取技术领域，具体是一种沉香提取工艺。
背景技术
沉香(Aloes)，古语写作“沈香”，是我国传统的名贵中药材，具有纳气平喘、消炎止痛的功效。国产沉香为瑞香科植物白木香在受到外界真菌侵害后产生的含树脂的木材，常被称为“木中钻石”。随着人工沉香的开发，沉香早已不再局限于入药，而是更多地提取沉香的化学成分，用于制作精油、熏香、面膜、纯露等居家用品。
当前对沉香的研究主要集中于化学成分的分析，鲜少有人对沉香的提取工艺进行优化，现有的沉香提取工艺中沉香利用率有待提高。
有鉴于此，本申请人针对现有技术中的上述缺陷深入研究，遂有本案产生。
发明内容
本发明的主要目的在于提供一种沉香提取工艺，其具有提高沉香浸提物含量的特点，工艺经济且简便。
为了达成上述目的，本发明的解决方案是：一种沉香提取工艺，包括：
将沉香破碎过80目筛，以0.01-0.1g/mL的浓度在萃取剂中冷浸，冷浸时间为24h-48h，再采用高效液相色谱仪对浸出液进行色谱分析；
其中，所述萃取剂为乙醇—三氯甲烷溶液，所述乙醇—三氯甲烷溶液浓度为40％，所用乙醇浓度为95％乙醇，所述三氯甲烷为分析纯；
所述沉香为虫漏人工沉香(白木香)结香4年。
进一步，冷浸后还包括进行回流，回流时间为2h。
进一步，所述沉香采用高速粉碎机进行破碎。
进一步，破碎过80目筛的沉香使用密封袋保存备用。
具体实施方式
为了进一步解释本发明的技术方案，下面通过具体实施例来对本发明进行详细阐述。
实施例一
一种沉香提取工艺，包括：
将沉香破碎过80目筛，以0.01-0.1g/mL的浓度在萃取剂中冷浸，冷浸时间为24h-48h，再采用高效液相色谱仪对浸出液进行色谱分析；
其中，所述萃取剂为乙醇—三氯甲烷溶液，所述乙醇—三氯甲烷溶液浓度为40％，所用乙醇浓度为95％乙醇，所述三氯甲烷为分析纯；
所述沉香为虫漏人工沉香(白木香)结香4年。
采用上述工艺后，通过对过筛的目数、提取方式、沉香样品质量与萃取剂体积的比值、萃取试剂及比值等进行优化，沉香浸提物总含量达 225.21g/kg，浸提物总含量比其他方法提高2.78倍，沉香四醇、2-(2- 苯乙基)色酮、2-(2-(4-甲氧基)苯乙基)色酮含量相较其他三种方法均达到了最高值，且该方法对沉香试样量要求低，在最大程度保留了沉香原有化学成分的同时，以经济、简便的方法显著提高了沉香浸提物含量。
本实施例中，先对沉香的目数进行了对比，沉香目数优化结果如表 1所示，由表中可知，目数对沉香浸提物、沉香四醇、2-(2-苯乙基)色酮、2-(2-(4-甲氧基)苯乙基)色酮含量有显著的影响，过80目筛的沉香化学成分考查指标数值均为最大，其中沉香浸提物总含量达到 194.32g/kg，20目的浸提物含量仅为80目的48.35％，且颗粒越小越有助于色酮类化合物的提取。较细的沉香样品有助于沉香化学成分的溶出。因过度粉碎容易产生粉尘颗粒，增加试样的消耗，且小颗粒样品在提取过程中容易聚集结块，因此选取最佳粉碎目数为80目。
表1沉香目数优化相关考查指标数值
然后，选定7个不同浓度的样品质量浓度进行优化，其结果如表3 所示。由表3可知，沉香化合物含量随着浓度的升高呈现下降的趋势，在0.01g/mL浓度下，沉香浸提物总含量为172.56g/kg，沉香四醇、2- (2-苯乙基)色酮、2-(2-(4-甲氧基)苯乙基)色酮含量也达最高；当样品浓度大于0.06g/mL，其4个指标维持相对的稳定。由于野生的沉香十分稀少，价格昂贵，所以，本申请中选取0.01g/mL的样品质量浓度作为沉香化合物提取的最佳浓度，在减少沉香试样的损耗的同时，提高沉香利用率，发挥沉香最大经济效益。
表3不同浓度沉香优化考查指标数值
不同沉香化学成分萃取剂对比：
天然药物沉香化学成分复杂多样，含有倍半萜、脂肪酸、色酮等多种挥发性、半挥发性和不易挥发性成分。本申请中选取了乙醇、甲醇、乙酸乙酯等8种试剂进行选择比较，结果如表4所示。由表可知，在一系列极性差异较大的试剂中，沉香化学物质提取含量最高的试剂为甲醇，乙醇次之，其含量可达甲醇的90.15％，而含量较低的试剂为石油醚、正己烷和乙醚等弱极性试剂。
表4沉香化合物提取剂考查指标数值
现有沉香化学成分的提取大多采用单化学剂，如采用提取量最高的甲醇作为提取剂，也有采用乙醚萃取并进行超声。本申请中结合沉香化学成分的差异性，选取乙醇和三氯甲烷作为提取剂，进一步探索不同比例的乙醇和三氯甲烷试剂对沉香化学成分提取的影响，其结果如表5所示。
由表5可知，40％的乙醇—三氯甲烷溶液浸提得到化合物总含量最高达197.33g/kg，且沉香四醇、2-(2-苯乙基)色酮、2-(2-(4-甲氧基) 苯乙基)色酮分别占最高含量的97.46％，93.61％和93.99％。故选取 40％的乙醇—三氯甲烷溶液(即40ml乙醇+60ml三氯甲烷)作为最佳提取剂。表5中，浓度90％表示：90ml乙醇+10ml氯仿混合溶液。
表5不同比例乙醇—三氯甲烷对沉香化学成分提取相关指标数值
进一步优化方案，所述沉香采用高速粉碎机进行破碎。
进一步优化方案，破碎过80目筛的沉香使用密封袋保存备用。
本申请以市售的人工沉香(虫养)为样品，通过对沉香的过筛的目数、提取方式、沉香样品质量与萃取剂体积的比值、萃取试剂及比值等进行优化，其最终结果如表6所示。
方法一、二和三分别参照中华人民共和国林业行业标准LY/T2904- 2017沉香、海南地方标准DB46/T421-2017沉香鉴定和2015版《中华人民共和国药典》对样品进行处理分析。
表6 4种方法提取沉香化学成分相关指标数值
本方法将沉香样品过80目筛，以0.01g/mL(m:v)的浓度在体积浓度40％的乙醇一三氯甲烷溶液冷浸24h后，沉香浸提物总含量达 225.21g/kg，浸提物总含量比方法一提高2.78倍，沉香四醇、2-(2- 苯乙基)色酮、2-(2-(4-甲氧基)苯乙基)色酮含量相较其他三种方法均达到了最高值，且该方法对沉香试样量要求低，在最大程度保留了沉香原有化学成分的同时，以经济、简俩的方法显著提高了沉香浸提物含量。
实施例二
与实施例一不同的是，冷浸后还包括进行回流处理，回流时间为2h。
当前对沉香化学成分提取的方法大多为回流和超声波两种，本实施例中选取了静置、超声和回流等5种方法对沉香的化学物质提取含量进行比对分析，4个考查指标数值如表2所示。
冷浸后回流，浸提物的总含量最高，沉香四醇、2-(2-苯乙基)色酮、 2-(2-(4-甲氧基)苯乙基)色酮含量也处于较高水平，该方法在不破坏沉香原有的成分的同时，也能减少易挥发性成分的损失。
上述实施例并非限定本发明的产品形态和式样，任何所属技术领域的普通技术人员对其所做的适当变化或修饰，皆应视为不脱离本发明的专利范畴。
Claims (4)
1.一种沉香提取工艺，其特征在于，包括：
将沉香破碎过80目筛，以0.01-0.1g/mL的浓度在萃取剂中冷浸，冷浸时间为24h-48h，再采用高效液相色谱仪对浸出液进行色谱分析；
其中，所述萃取剂为乙醇—三氯甲烷溶液，所述乙醇—三氯甲烷溶液浓度为40％，所用乙醇浓度为95％乙醇，所述三氯甲烷为分析纯；
所述沉香为虫漏人工沉香(白木香)结香4年。
2.如权利要求1所述的沉香提取工艺，其特征在于，冷浸后还包括进行回流，回流时间为2h。
3.如权利要求1所述的沉香提取工艺，其特征在于，所述沉香采用高速粉碎机进行破碎。
4.如权利要求1所述的沉香提取工艺，其特征在于，破碎过80目筛的沉香使用密封袋保存备用。
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| 马永青;袁丽华;刘永利;: "沉香化学成分与分析方法研究进展", 沈阳药科大学学报 * |
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