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中国精品科技期刊2020
宋道光, 徐顺连, 樊鑫宇, 陈志. 高速逆流色谱法分离制备小叶金钱草中杨梅苷与槲皮苷[J]. 食品工业科技, 2019, 40(11): 265-269,283. DOI: 10.13386/j.issn1002-0306.2019.11.044
引用本文: 宋道光, 徐顺连, 樊鑫宇, 陈志. 高速逆流色谱法分离制备小叶金钱草中杨梅苷与槲皮苷[J]. 食品工业科技, 2019, 40(11): 265-269,283. DOI: 10.13386/j.issn1002-0306.2019.11.044
SONG Dao-guang, XU Shun-lian, FAN Xin-yu, CHEN Zhi. Isolation and Preparation of Myricitrin and Quercitrin from Hydrocotyle sibthorpioides Lam. by High-speed Counter-current Chromatography[J]. Science and Technology of Food Industry, 2019, 40(11): 265-269,283. DOI: 10.13386/j.issn1002-0306.2019.11.044
Citation: SONG Dao-guang, XU Shun-lian, FAN Xin-yu, CHEN Zhi. Isolation and Preparation of Myricitrin and Quercitrin from Hydrocotyle sibthorpioides Lam. by High-speed Counter-current Chromatography[J]. Science and Technology of Food Industry, 2019, 40(11): 265-269,283. DOI: 10.13386/j.issn1002-0306.2019.11.044

高速逆流色谱法分离制备小叶金钱草中杨梅苷与槲皮苷

Isolation and Preparation of Myricitrin and Quercitrin from Hydrocotyle sibthorpioides Lam. by High-speed Counter-current Chromatography

  • 摘要: 应用高速逆流色谱法对小叶金钱草中的杨梅苷和槲皮苷进行分离制备。小叶金钱草乙醇提取物依次经石油醚、乙酸乙酯、正丁醇萃取,取乙酸乙酯萃取物经葡聚糖凝胶75%甲醇洗脱纯化,高速逆流色谱正己烷-正丁醇-水(1.75:1:1,v:v)两相溶剂系统分离,以上相为固定相,下相为流动相,在主机转速900 r/min,流速2 mL/min,检测波长254 nm条件下进行分离制备,并将所得产物进行高效液相检测和1H、13C NMR结构分析。结果表明,该条件下经一步分离可同时得到18.63和17.49 mg的两种产物,其纯度为97.85%和95.42%,经1H、13C NMR分析确定其为杨梅苷和槲皮苷。

     

    Abstract: High-speed counte-current chromatography(HSCCC)was developed for separation and purification of myricitrin and quercitrin from Hydrocotyle sibthorpioides Lam(HSL). The HSL ethanol extracts was extracted successively with petroleum ether,ethyl acetate and n-butanol. The ethyl acetate fraction was purified by Sephadex LH-20 elution with 75% methanol,and separated by high-speed countercurrent chromatography of n-hexane-n-butanol-water(1.75:1:1,v:v)two-phase solvent system,in which the upper phase as stationary phase and the lower phase was used as the mobile phase,at a flow rate of 2.0 mL/min.The rotation speed and detection wavelength were set at 900 r/min and 254 nm,respectively. The obtained product was subjected to high performance liquid phase detection and 1H,13C NMR structural analysis. Results showed that,under this separation conditions,two products of 18.63 and 17.49 mg were obtained in one step,and the purity was 97.85% and 95.42%,respectivty,which were determined to be myricetin and quercetin by 1H and 13C NMR.

     

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