丹参综合提取分离及丹参酮ⅡA磺酸钠制备工艺研究

Study on Integrated Extraction of Effective Components from Salvia miltiorrhiza Bunge and Preparation of Tanshinone ⅡA Sodium Sulfonate

本研究以陕西商洛所产丹参为原料,对丹参中主要有效成分的同步综合提取工艺进行了优化。优化后的提取工艺为:乙醇浓度为80%,料液比为1∶25,提取时间3h,提取温度60℃。提取液浓缩至比重1.05后加入4倍量(mL/g)的水沉淀,过滤,将水溶性成分和脂溶性成分分离。水液以大孔树脂吸附,水洗脱,得到丹参素和原儿茶醛的水洗液。水洗脱后的树脂以40%的乙醇洗脱,收集乙醇洗脱液得到丹酚酸B;提取浓缩液水沉后的沉淀干燥,以苯溶解,过滤,滤液以中性氧化铝柱层析,得到各种单体成分。优化后的纯化工艺各成分的得率为:原儿茶醛3.6%,丹参素1.2%,丹酚酸B5.5%,丹参酮I 0.23%,丹参酮ⅡA 3.8%,丹参酮IIB 0.72%,隐丹参酮0.18%,丹参酸甲酯0.09%;含量分别为:98.3%,99.2%,91.7%,97.2%,98.8%,98.5%,97.6%,98.3%。以配料比、反应时间、反应温度和溶液碱度为影响因素,采用最陡坡实验法对水溶性化合物丹参酮ⅡA磺酸钠的制备工艺进行了优化,得率为86.2%,含量为96.7%。

In this study, the synchronous integrated extraction of the effective components from Salvia miltiorrhiza was op- timized. The optimum extraction condition was：80% as ethanol concentration,1： 25 as ratio of solid to liquid,3 h as ex- traction time,60 ℃ as extraction temperature. The extract was then concentrated to the proportion of 1.05 followed by adding 4 times amount （mL/g） of water for sedimentation. The water-soluble fraction and sediment were then separated. The water-soluble fraction was applied to macroporous resin adsorption, elution, to afford two sub-fractions, containing Danshensu and protocatechuic aldehyde,respectively. The macroporous resin was further eluted with 40% ethanol to af- ford salvianolic acid B. The sediment was dried and dissolved in benzene. It was then filtrated and applied to neutral alu- mina column chromatography to afford each single component. The yields of the purified components using the optimized purification process were： protocatechuic aldehyde 3.6%, Danshensu 1.2%, salvianolic acid B 5.5%, tanshinone I 0.23% ,tanshinone Ⅱ A 3.8% ,tanshinone ⅡB 0.72%, cryptotanshinone 0.18% ,salvia acid methyl ester 0.09%. Their respective purities were：98.3% ,99.2% ,91.7% ,97.2% ,98.8% ,98.5% ,97.6% and 98.3%. The preparation process of water soluble compound, tanshinone A sulfonate, was optimized by the steep slope experiment using mixture ratio, reaction time, reaction temperature, solution alkalinity as influencing factors. The yield and content were determined to be 86.2% and 96.7% ,respectively.