pH-zone-refining counter-current chromatography,rosmarinic acid,salvianolic acid B,"/> 区带逆流色谱法分离纯化丹参中的丹酚酸B和迷迭香酸

山东科学 ›› 2016, Vol. 29 ›› Issue (3): 13-17.doi: 10.3976/j.issn.1002-4026.2016.03.003

• 中药与天然活性产物 • 上一篇    下一篇

区带逆流色谱法分离纯化丹参中的丹酚酸B和迷迭香酸

李怀志,宫成玉,李云,杨鹏,李佳,王晓   

  1.  1.山东中医药大学药学院,山东济南250355; 2.烟台出入境检验检疫局,山东烟台264000; 3.济南三峰生物工程有限责任公司,山东济南250014; 4.山东省中药质量控制技术重点实验室,山东省分析测试中心,山东济南250014
  • 收稿日期:2016-02-22 出版日期:2016-06-20 发布日期:2016-06-20
  • 通信作者: 王晓(1971-),男,研究员。Email:wangx@sdas.org E-mail:wangx@sdas.org
  • 作者简介:李怀志(1991-),女,硕士研究生,研究方向为天然产物与纯化。
  • 基金资助:

    山东省科技发展计划(2014GZX219003)

Separation and purification of salvianolic acid B and rosmarinic acid from Salvia miltiorrhiza Bge. by pH-zone-refining counter-current#br# chromatography
 

LI Huai-zhi, GONG Cheng-yu , LI Yun, YANG Peng, LI Jia , WANG Xiao   

  1. 1.School of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250355, China;  2. Yantai Entry exit Inspection and Quarantine Bureau, Yantai 264000, China; 3. Sanfeng Biological Engineering Technology Co. Ltd. ,Jinan 250014, China;  4. Shandong Provincial Key Laboratory of Traditional Chinese Medicine QualityControl Technology, Shandong Analysis and Test Center, Jinan
    250014, China
  • Received:2016-02-22 Online:2016-06-20 Published:2016-06-20

摘要:

 采用pH区带精制逆流色谱技术(pH-ZRCCC)快速分离纯化丹参中的丹酚酸B和迷迭香酸?以乙酸乙酯-(11,V/V)为溶剂体系,上相加入三氟乙酸,使浓度达到10 mmol/L,作为固定相;下相加入氨水使浓度达到20 mmol/L,作为流动相;设置主机转速为850 r/min,流速为2.0 mL/min,检测波长为280 nm,对样品进行分离制备?从500 mg丹参粗提物中一次分离得到386 mg丹酚酸B以及25 mg迷迭香酸,HPLC分析纯度分别为96.3%98.1%,各化合物通过电喷雾电离(ESI)谱和1H-NMR进行了化学结构鉴定?研究结果表明,pH-ZRCCC是一种快速?高效分离纯化丹酚酸B和迷迭香酸的方法

关键词: 丹酚酸B, pH区带逆流色谱, 迷迭香酸

Abstract:

We rapidly separated and purified salvianolic acid B and rosmarinic acid from Salvia miltiorrhiza Bge. By pHzonerefining countercurrent chromatography ( pH-ZRCCC) . The extraction conditions included solvent system of ethyl acetatewater ( 11, V/ V) , upper stationary phase of 10 mmol/ L trifluoroacetic acid, lower mobile phase of 20 mmol/ L NH 3 H 2 O, rotation speed of 850 r/ min, flow speed of 2. 0 mL/ min, and detection wavelength of 280 nm. Salvianolic acid B of 386 mg and rosmarinic acid of 25 mg were extractedfrom crude extract of 500 mg, whose purities were 96. 3% and 98.1% through HPLC analysis. Their compound structures were identified by ESIMS and 1 HNMR. Experimental results show that pHZRCCC is a rapid and efficient method to separate and purify salvianolic acid B and rosmarinic acid.

Key words: pH-zone-refining counter-current chromatography')">pH-zone-refining counter-current chromatography, rosmarinic acid, salvianolic acid B

中图分类号: 

  • 引用本文

    李怀志,宫成玉,李云,杨鹏,李佳,王晓. 区带逆流色谱法分离纯化丹参中的丹酚酸B和迷迭香酸[J]. 山东科学, 2016, 29(3): 13-17.

    LI Huai-zhi,GONG Cheng-yu,LI Yun,YANG Peng, LI Jia, WANG Xiao.

    Separation and purification of salvianolic acid B and rosmarinic acid from Salvia miltiorrhiza Bge. by pH-zone-refining counter-current#br# chromatography
     [J]. SHANDONG SCIENCE, 2016, 29(3): 13-17.