【作者】 李国章；

【导师】 饶力群； 曹庸；

【作者基本信息】 湖南农业大学 ， 植物学， 2006， 硕士

【摘要】 丹参是我国传统重要中药，具有活血化淤、理气止痛之功效，其各种制剂被广泛用于心脑血管病的治疗。丹参的主要功能成分为脂溶性的丹参酮和水溶性的原儿茶醛、丹参素。丹参酮又包括丹参酮ⅡA、丹参酮Ⅰ、隐丹参酮等。近年来，丹参类药用量增大，市场对丹参的活性成分丹参酮，特别是丹参酮ⅡA的需求量也在不断增大。如何采取先进工艺从丹参中提取纯化丹参酮ⅡA，取得更好的经济效益，已成为相关厂商出资研究的热点。围绕丹参酮ⅡA的提取和纯化，本论文中的研究做了如下工作：1．采用超临界CO₂流体萃取技术从丹参中萃取丹参酮ⅡA。研究了萃取压力、萃取温度、CO₂流量、夹带剂用量对萃取率的影响；通过正交试验，得到优化的萃取条件：萃取压力：25 MPa，萃取温度45℃，CO2流量30 kg·h^-1，夹带剂流量为1.2 mL·min^-1，在该条件下，丹参酮ⅡA的萃取率达87.2％，比报道的最高值85.7％提高了1.5％。2．对萃取丹参酮时使用的夹带剂种类和用量进行了比较研究。分别用不同流量的乙醇（95％，V／V）、丙酮、正辛烷作夹带剂，以3种丹参酮的萃取率为指标，比较3种夹带剂的效果。结果显示，乙醇作夹带剂比丙酮和正辛烷好。3．通过对吸附剂和洗脱剂的选择，改进了丹参酮ⅡA柱层析纯化方法。用改进的柱层析方法纯化丹参酮粗产品得到纯度为89.15％的丹参酮ⅡA，回收率为30.97％，与同类方法相比，该方法简洁易行，得到的丹参酮ⅡA纯度也较好，但还存在回收率较低的问题。4．利用结晶重结晶方法进一步对丹参酮ⅡA粗产品进行纯化研究。研究了不同溶剂用量对丹参酮ⅡA纯度和回收率的影响；研究了不同重结晶温度对丹参酮ⅡA纯度和回收率的影响；以丹参酮ⅡA的纯度和回收率为指标，研究得到了用结晶重结晶方法纯化丹参酮ⅡA较佳工艺：用5倍量的溶剂A溶解丹参总酮，1.4倍量的溶剂B滴加，冷藏、过滤、干燥，得产品1，用溶剂C溶解产品1，于25℃—45℃保温析晶，过滤干燥得到的丹参酮ⅡA，纯度最高达96.3％，回收率最高达76.6％。用该方法得到的丹参酮ⅡA纯度高，提取率也较高，且工艺流程短，成本低，周期短，节省能耗，是目前从丹参总酮中纯化丹参酮ⅡA的最好的方法之一。更多还原

【Abstract】 Tanshin （Salvia Miltiorrhiza Bunge） is one of the most importantChinese traditional medicine. It can activate blood circulation to dissipateblood stasis and regulate the flow of qi to alleviate pain. Lots of itsmedicaments are widely used to heal angiocardiopathy andcerebrovascular disease. Several principal ingredients of Tanshin arefat-soluble Tanshinones, such as Tanshinone-ⅡA, Tanshinone-ⅠandCriptotanshinone, as well as water-soluble Protocatechualdehyde andDanshensu. Demand for Tanshin medicaments has increased, andrelatively demand for TanshinoneⅡ-A, which is one of its key bioactivecomponents, has also increased rapidly in recent years. Therefore,concerned enterprises are engaged in developing advanced technologicalprocess of extraction and purification in word to profit greatly. Followingis a summary of the work performed in my study on the extraction andpurification of TanshinoneⅡ-A from Tanshin.1. Tanshinone-ⅡA was extracted from Tanshin material bysupercritical CO₂ fluid extraction technology （SCFET）. The influencesof extraction pressure, extraction temperature, CO₂ flux and entrainer fluxwere investigated. Optimized parameters of SCFET were obtainedthrough orthogonal experiment. The results were as follows: Theextraction pressure was at 25 MPa, the extraction temperature was at45℃, the CO₂ flux was 30 kg·h^-1 and the entrainer flux was 1.2 mL·min^-1. under this condition, the extraction rate of Tanshinone-ⅡA reached to87.2%, higher by 1.5% than 87.2% to which the lectures reported thatreached.2. The effect of three kinds of entrainers （ethanol, acetone andnomal octane）on Tanshinones were studied. Taking the extraction rate asstandard, three kinds of entrainers were pumped into the equipment tohelp extract TanshinoneⅡ-A at different flux and the effect onTanshinones were compared. The results showed that ethanol is the best.3. Through choosing the suitable sorbent and eluant, the method ofcolumn chromatography to purify Tanshinone-ⅡA from overallTanshinones was mended, was purifid to obtain pure Tanshinone-ⅡA Bythis method, mended, were choosed by experiment. Solubility ofTanshinones in twelve kinds of solvent was also tested. The purity andrecovery of TanshinoneⅡ-A obtained by the mended method were89.15% and 30.97%, the purify was higher whereas the recovery waslower. Comparing with similar other method, this method is simple andpractical.4. Tanshinone-ⅡA was purifid from overall Tanshinones to obtainpure Tanshinone-ⅡA by crystal and recrystal means. The influences of theamount of solvent on the purify and recovery of Tanshinone-ⅡA werestudied. The influences of recrystal temperature on the purify andrecovery of Tanshinone-ⅡA were also studied. Taking the purify andrecovery of Tanshinone-ⅡA as standard, the optimized technologicalprocess by which Tanshinone-ⅡA was purified was obtained. Dissolvingoverall Tanshinone by solvent A at material-solvent ratio 1: 5, titrating by 1.4 times of solvent B, refrigerating the solution, filtrating, desiccating,product numble one was obtained. Dissolving product number one bysolvent C, recrystallizing Tanshinone-ⅡA, filtrating, desiccating, productnumber two was obtained, Its purify and recovery of Tanshinone-ⅡAwere up to 96.3% and 76.6%. By this method, both purify and recoveryof Tanshinone-ⅡA are high, and the process was simple, low-cost, energysaving. It is one of the best methods of purifying Tanshinone-ⅡA at thepresent time.更多还原