高速逆流色谱法从小叶金钱草中分离四种黄酮苷类化合物  

Separation of Four Flavonoid Glycosides from Hydrocotyle sibthorpioides Lam.by High-speed Counter-current Chromatography

作　　者：宋道光 陈志 SONG Daoguang;CHEN Zhi(School of Geography Science,Qinghai Normal University,Xining 810008,China;Key Laboratory of Medicinal Animal and Plant Resources of the Qinghai-Tibetan Plateau,Qinghai Normal University,Xining 810008,China)

机构地区：[1]青海师范大学地理科学学院,青海西宁810008 [2]青海师范大学,青藏高原药用动植物资源重点实验室,青海西宁810008

出　　处：《食品工业科技》2022年第24期93-101,共9页Science and Technology of Food Industry

基　　金：青藏高原药用动植物资源重点实验室(2017-ZJ-Y13)。

摘　　要：为研究小叶金钱草中大极性黄酮苷类化合物,采用正丁醇萃取、DM 301大孔吸附树脂、葡聚糖凝胶、反相硅胶柱层析纯化,得到大极性黄酮苷类组分。结合离线二维高速逆流色谱,分别以正己烷/正丁醇/水/冰乙酸(系统Ⅰ:1:2:1:0.1,v/v/v/v和系统Ⅱ:1:1:1:0.1,v/v/v/v)为溶剂系统,在主机转速900 r/min、流速2 mL/min、254 nm检测波长条件下进行分离。结果表明,从小叶金钱草正丁醇组分中分离得到四种黄酮苷类化合物,经^(1)H、^(13)C NMR鉴定为杨梅素3,3'-二-α-L-鼠李糖苷(1)、木犀草素-7-O-β-D-葡萄糖醛酸苷(2)、槲皮素3,3'-二-α-L-鼠李糖苷(3)和芹菜素-7-O-β-D-葡萄糖醛酸苷(4),高效液相色谱分析其纯度均大于95%。化合物3为首次从小叶金钱草中分离得到,本研究为小叶金钱草的化学成分研究提供依据。For an improved study of flavonoid glycosides of great polarity from Hydrocotyle sibthorpioides Lam(HSL),the large polar flavonoid glycosides were extracted with n-BuOH,purified by DM 301 macroporous resin,Sephadex LH-20 and reversed-phase silica gel(ODS/RP-18).Combined with offline two-dimensional high-speed counter-current chromatography(HSCCC),the fraction with the target compounds was purified by HSCCC adopting a two-phase solvent system consisting of n-hexane/n-BuOH/water/glacial acetic acid(system Ⅰ:1:2:1:0.1,v/v/v/v and system Ⅱ:1:1:1:0.1,v/v/v/v).Additionally,the rotation velocity,and flow rate in conjunction with detection wavelength were adjusted to 2.0 mL/min,900 r/min,and 254 nm respectively.The results demonstrated that four compounds were isolated from HSL,whose structures were determined as myricetin 3,3'-di-α-L-rhamnopyranoside(1),luteolin-7-O-β-D-glucuronide(2),quercetin 3,3'-di-α-L-rhamnopyranoside(3)and apigenin 7-O-β-D-glucuronide(4)operating ^(1)H NMR and ^(13)C NMR spectroscopy.The purity of the four compounds were above 95%by HPLC analysis,and compound 3 was isolated from the HSL for the first time.Thus,this work would provide a basis for the study of the chemical constituents of HSL.

关 键 词：小叶金钱草 槲皮素鼠李糖苷 黄酮苷 高速逆流色谱 梯度洗脱 

分 类 号：R284.1[医药卫生—中药学]