高速逆流色谱法分离纯化青皮中六种多甲氧基黄酮

Isolation and Purification of Six Polymethoxyflavones from Pericarpium citri Reticulatae Viride by High-speed Counter-current Chromatography

应用高速逆流色谱法(HSCCC)分离制备了青皮中6种多甲氧基黄酮类(Polymethoxyflavones,PMFs)化合物。以正己烷-乙酸乙酯-甲醇-水(体积比为4∶6∶4∶6)为两相溶剂系统,在主机转速800 r/min、流动相流速2mL/min、检测波长254 nm条件下进行分离制备,460 min内从270 mg青皮粗提物中一步分离制备得到甜橙素(1,sinensetin)3.5 mg,5,7,8,4-四甲氧基黄酮(2)13.9 mg,川陈皮素(3,Nobiletin)51.3 mg,3,5,6,7,8,3′,4′-七甲氧基黄酮(4)9.5 mg,橘皮素(5,Tangeretin)44.7 mg,5-去甲川陈皮素(6,5-O-DesmethylNobiletin)11.2 mg,纯度均达97%以上,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。利用该方法可以对青皮中的黄酮类化合物进行快速的分离和纯化。

Six Polymethoxyflavones were prepared, isolated and purified from Pericarpium citri Reticulatae Yiride by highspeed counter-current chromatography （ HSCCC ） . A two-phase solvent system composed of n-hexane-ethyl acetatemethanol-water （ 4： 6： 4：6 ,v / v / v / v ） was used. With in 460 minuets ,3.5 mg of sinensetin, 13.9 mg of 5,7,8,4＇- tetramethoxy flavone, 51.3 mg of nobiletin, 9.5 mg of 3,5,6,7,8,3＇,4＇-heptamethoxyflavone, 44.7 mg of tangeretin and 11.2 mg of 5-O-DesmethylNobiletin with their purities over 97.0% were obtained from 270 mg of the crude extract of Pericarpium cirri Reticulatae Viride in one - step elution under the conditions of a flow rate of 2 mL. mint ,800 r. min^-1 and the detection wave length of 254 nm. The obtained fractions were analyzed by high performance liquid chromatography （HPLC）, and identified by mass spectrometry （MS）, ^1H NMR and ^13C NMR. The results indicate that HSCCC is a powerful technique for the purification of Polymethoxyflavones from Pericarpium citri Reticulatae Viride.