Peng Jinyong, Fan Guorong, Wu Yutian
Shanghai Key Laboratory for Pharmaceutical Metabolite Research, School of Pharmacy, Second Military Medical University, No. 325 Guohe Road, Shanghai 200433, China.
J Chromatogr A. 2005 Oct 14;1091(1-2):89-93. doi: 10.1016/j.chroma.2005.07.072.
A preparative high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of ethyl acetate-n-butanol-water (2:7:9, v/v/v) was successfully performed to isolate and separate clemastanin B and indigoticoside A from the plant of Radix Isatidis, a traditional Chinese medicine. A total of 59.2 mg clemastanin B and 66.1 mg indigoticoside A with purities of 94.6% and 99.0% determined by high performance liquid chromatography (HPLC) were obtained in one-step elution from 250 mg crude extract, which contained clemastanin B 24.8% and indigoticoside A 28.4%, and the recoveries of clemastanin B and indigoticoside A were 90.3% and 92.2%, respectively. The chemical structure was identified by IR, MS, 1H NMR and 13C NMR.
采用由乙酸乙酯 - 正丁醇 - 水(2:7:9,v/v/v)组成的两相溶剂系统的制备型高速逆流色谱(HSCCC),成功地从传统中药板蓝根中分离出了马蓝苷B和靛玉红苷A。从250 mg粗提物(其中马蓝苷B含量为24.8%,靛玉红苷A含量为28.4%)中一步洗脱,通过高效液相色谱(HPLC)测定,共获得了59.2 mg纯度为94.6%的马蓝苷B和66.1 mg纯度为99.0%的靛玉红苷A,马蓝苷B和靛玉红苷A的回收率分别为90.3%和92.2%。通过红外光谱(IR)、质谱(MS)、氢核磁共振(1H NMR)和碳核磁共振(13C NMR)对其化学结构进行了鉴定。