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作 者:贺天雨 王尉[1,2] 徐双双[1,2] 赵新颖[1,2] 张经华[1,2]
机构地区:[1]北京市理化分析测试中心,北京100089 [2]有机材料检测技术与质量评价北京市重点实验室,北京100094
出 处:《现代科学仪器》2017年第1期65-70,共6页Modern Scientific Instruments
摘 要:目的:建立一种快速高效的制备分离红景天中红景天苷与酪醇的方法。方法:采用高速逆流色谱法对红景天乙醇提取物中的红景天苷和酪醇进行富集,溶剂体系为正丁醇:乙酸乙酯:水(2:3:5),仪器转速900r/min,流速2mL/min,检测波长254nm。对富集后的样品进行半制备液相色谱二次纯化,流动相为甲醇-水,流速4mL/min,检测波长275nm。通过紫外-可见光谱、红外光谱、质谱、核磁共振波谱对红景天苷和酪醇进行了结构确证。结论:该方法操作简单、制备量大、纯度高,可为新药研究和工业化生产提供参考。Objective: A rapid and efficient method for preparation of Salidroside and Tyrosol from Rhodiola crenulata was established. Methods: Salidroside and tyrosol in the Rhodiola crenulata ethanol extract were enriched by using HSCCC with N-butanol: ethyl acetate: water (2: 3: 5)as the solvent system, The flow rate was 2mL/min while the apparatus rotated at 900 r/min and the detection wavelength was at 254 nm. The concentrate was purified by semi- preparative liquid chromatography furtherly. The mobile phase consisted of methanol-water, the flow rate was 4 mL/min, and the detection wavelength was 275nm. The structures of salidroside and tyrosol were confirmed by UV-Vis, IR, MS and NMR spectroscopy. Conclusion: The method that has the advantages of simple operation, large preparation volume and high purity can provide reference for new drug research and industrial production.
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