摘要
应用聚酰胺柱层析法和高效制备液相色谱法研究黄蜀葵花(Abelmoschus manihot(L.)Medicus)中金丝桃苷及其异构体分离制备方法。结果表明:黄蜀葵花粗提物经聚酰胺柱层析分离后,50%乙醇洗脱液中可得到金丝桃苷及其异构体的混合物,将混合物冻干后经高效制备液相色谱分离,高效制备液相柱为Calesil A-120(250 mm×21.2 mm,10μm),流动相为乙腈-0.2%乙酸(15∶85,V/V),上样量20.0 mg,流速25.0 m L/min,柱温30℃,检测波长280 nm,得到纯度分布在99%和97%以上的两种纯物质。经核磁共振及质谱分析,鉴定其分别为金丝桃苷和异槲皮苷,二者互为立体异构体。
Polyamide chromatography and preparative high performance liquid chromatography(HPLC) were used for the separation and preparation of two isomers of hyperoside from Abelmoschus manihot(L.) Medicus flowers. The results indicated that the 50% ethanol eluate contained a mixture of hyperoside and its isomers after polyamide chromatography. Then the freeze-dried mixture was separated by preparative HPLC on Calesil A-120 column(250 mm × 21.2 mm, 10 μm) with acetonitrile-0.2% aqueous acetic acid(15:85, V/V) as the mobile phase by injecting 20.0 mg of the sample at a flow rate of 25.0 m L/min; the column temperature was 30 ℃, and detection wavelength was 280 nm. Two isomers were achieved and identified by MS, 1H and 13 C NMR as hyperoside and isoquercitrin with purities of more than 99% and 97%, respectively, and both were stereoisomer.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2015年第4期131-135,共5页
Food Science
基金
北京市自然科学基金重点项目(KZ201410011016)
关键词
黄蜀葵花
聚酰胺柱层析
高效制备液相色谱
金丝桃苷
异槲皮苷
Abelmoschus manihot(L.) Medicus
polyamide chromatography
preparative high performance liquid chromatography
hyperoside
isoquercitrin
