摘要
应用高速逆流色谱法(HSCCC)分离纯化连翘果实中的两对木脂素类立体异构体。分别用乙酸乙酯-正丁醇-甲醇-水(体积比5∶0.7∶1∶5)和乙酸乙酯-正丁醇-甲醇-水(体积比5∶0.5∶1∶5)为两相溶剂体系,在转速为800 r/min、流速为1.5 mL/min、检测波长为254 nm的条件下进行分离,所得馏分经高效液相色谱(HPLC)检测纯度,电喷雾电离质谱(ESI-MS)和碳核磁共振波谱(13C NMR)鉴定化合物的结构。
Two pairs of stereomeric lignan,namely(+) pinoresinol monomethyl ether-β-D-glucoside and phillyrin,(+) pinoresinol-β-D-glucoside and(+) epipinoresinol-β-D-glucoside,were successfully isolated and purified from the fruits of Forsythia suspensa by high-speed counter-current chromatography(HSCCC) using two-phase solvent systems with composed of ethyl acetate-n-butanol-methanol-water(5∶0.7∶1∶5,volume ratio) and ethyl acetate-n-butanol-methanol-water(5∶0.5∶1∶5,volume ratio),respectively.The purities of the isolated compounds were all above 97 % determined by high-performance liquid chromatography(HPLC) and their structures were confirmed by electrospray ionization MS(ESI-MS),1HNMR,and 13CNMR.
出处
《林产化学与工业》
EI
CAS
CSCD
北大核心
2011年第5期41-47,共7页
Chemistry and Industry of Forest Products
基金
山东省科技攻关项目(2010GSF10287)
山东大学高校院所自主创新计划(201004010)
国家高科技研究发展计划(2010AA101605-05)
关键词
高速逆流色谱
连翘
立体异构体
high-speed counter-current chromatography
Forsythia suspensa
stereomer