天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (9): 1510-1516.

• 开发研究 • 上一篇    下一篇

丹参综合提取分离及丹参酮ⅡA磺酸钠制备工艺研究

李玉山*,王经安   

  1. 西安惠丰生化有限公司,西安 710075
  • 出版日期:2014-09-30 发布日期:2014-11-02

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

LI Yu-shan*, WANG Jing-an   

  1. Xi’An hui feng Biochemistry Co.,LTD,Xi’an 710075,China
  • Online:2014-09-30 Published:2014-11-02

摘要: 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%。

关键词: 丹参, 综合提取, 丹参酮IIA磺酸钠, 酚酸类化合物, 二萜醌类, 纯化

Abstract: In this study,the synchronous integrated extraction of the effective components from Salvia miltiorrhiza was optimized.The optimum extraction condition was:80% as ethanol concentration,1:25 as ratio of solid to liquid,3 h as extraction 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 afford salvianolic acid B.The sediment was dried and dissolved in benzene.It was then filtrated and applied to neutral alumina 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 II B 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.

Key words: Salvia miltierrhiza Bunge, comprehensive extraction, tanshinone II A sodium sulfonate, phenolic compounds, two terpene quinones, purification

中图分类号: 

TQ351.0