摘要
应用高速逆流色谱法分离制备了陈皮中3种黄酮类化合物。以石油醚-乙酸乙酯-甲醇-水(体积比为2∶4∶3∶3)为两相溶剂系统,在主机转速850r/min、流动相流速1.7mL/min、检测波长280nm条件下进行分离制备,6h内从4.0g陈皮粗提物中一步分离制备得到橙皮苷10.1mg、桔皮素49.8mg和5-羟基-6,7,8,3′,4′-五甲氧基黄酮50.6mg,纯度均达97.0%以上,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。利用该方法可以对陈皮中的黄酮类化合物进行快速的分离和纯化。
Three flavones were prepared,isolated and purified from Pericarpium Citri Reticulatae by high-speed counter-current chromatography(HSCCC).A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water(2∶4∶3∶3,v/v/v/v) was used.Within 6 hours,10.1 mg of heseridin,49.8 mg of 5,6,7,8,4′-pentamethoxyflavone and 50.6 mg of 5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone with their purities over 97.0% were obtained from 4.0 g of the crude extract of Pericarpium Citri Reticulatae in one-step elution under the conditions of a flow rate of 1.70 mL/min,800 r/min and the detection wavelength of 280 nm.The obtained fractions were analyzed by high performance liquid chromatography(HPLC),and identified by mass spectrometry(MS),1H-nuclear magnetic resonance(NMR) and13C-NMR.The results indicate that HSCCC is a powerful technique for the purification of flavones from Citrus reticulata Blanco.
出处
《色谱》
CAS
CSCD
北大核心
2009年第2期244-247,共4页
Chinese Journal of Chromatography
基金
泰安市科技发展计划[2007]10
关键词
高速逆流色谱
橙皮苷
桔皮素
5-羟基-6
7
8
3
′4′-五甲氧基黄酮
陈皮
high-speed counter-current chromatography(HSCCC)
hesperidin
5,6,7,8,4′-pentamethoxyflavone
5-hydroxy-6,7,8,3′,4′-pentamethoxyflavone
Pericarpium Citri Reticulatae