摘要
在静态吸附-解吸、动态吸附-解吸实验的基础上,对比了AB-8和D101大孔吸附树脂、聚酰胺树脂-1号(PLA-1)和聚酰胺树脂-2号(PLA-2)对竹柏总黄酮及穗花杉双黄酮的吸附-解吸性能,并对筛选出的AB-8型大孔吸附树脂纯化竹柏总黄酮的工艺进行探讨。在实验设计范围内,最佳工艺条件为:上样液中总黄酮质量浓度为1.5~3.0 g/L、上样流速22 mL/h、上样量220 mL;洗脱剂为体积分数80%的乙醇、洗脱流速44 mL/h、洗脱剂用量140 mL;竹柏总黄酮质量分数从13.6%提高到52.8%,穗花杉双黄酮质量分数从0.1%提高到2.37%。采用多种色谱分离纯化技术,从竹柏叶提取物的正丁醇萃取物中分离得到8个单体化合物,借助UV、FT-IR、MS、1H NMR及13C NMR鉴定出化合物的结构分别为:儿茶素(1)、芹菜素(2)、表儿茶素(3)、牡荆苷(4)、牡荆苷鼠李糖苷(5)、穗花杉双黄酮(6)、罗汉松双黄酮A(7)和白果黄素(8)。其中化合物4、5和8为首次从竹柏属植物中分离得到。
Based on the adsorption-desorption tests of total flavonoids and amentoflavone from leaves of Nageia nagi(Thunberg)Kuntze on different resins,AB-8 resin with the preferable adsorption and desorption performances was selected from four kinds of resins,which were AB-8 and D101 resins,and polyamide resins(PLA-1 and PLA-2).The optimum process was recommended as follows:for the adsorption tests,the mass concentration of total flavonoids was 1.5-3.0 g/L,the load rate was 22 mL/h and volume of loading solution was 220 mL;desorption tests was sequentially operated with 140 mL 80%ethanol-water solution as eluent at the wash rate of 44 mL/h.As a result,with the optimized processes,the content of total flavonoid and amentoflavone was significantly increased from 13.6%to 52.8%and 0.1%to 2.37%,respectively.Varieties of chromatographic techniques were used to separate and purify the extract fromleaves of N.nagi.The structures of the compounds were identified by UV,FT-IR,MS,1D NMR and 2D NMR.Eight compounds were isolated from the n-butanol extract from branches and leaves of N.nagi alcohol extract.They were catechin(1),apigenin(2),epi-catechin(3),vitexin(4),vitexin rhamnoside(5),amentoflavone(6),podocarpus flavone A(7),and bilobetin(8).Among them,compounds 4,5 and 8 were isolated from genus Nageia for the first time.
作者
郭婕
王欢
张祁
宋科
GUO Jie;WANG Huan;ZHANG Qi;SONG Ke(Key Laboratory of Hunan Forest Product and Chemical Industry Engineering,Jishou University,Zhangjiajie 427000,China)
出处
《林产化学与工业》
CAS
CSCD
北大核心
2021年第3期85-94,共10页
Chemistry and Industry of Forest Products
基金
国家自然科学基金资助项目(31560105,32060326)。
关键词
竹柏叶
总黄酮
双黄酮
黄酮碳苷
大孔树脂纯化
Nageia nagi leaves
flavonoids
biflavones
flavone glycosides
purification with macroporous resin
