[关键词]
[摘要]
目的 建立对荷叶生物碱进行分离的pH区带逆流色谱方法。方法 溶剂系统为叔丁基甲醚-甲醇-水(4∶1∶5),上相添加三乙胺(10 mmol/L)作为固定相,下相添加盐酸(5 mmol/L)为流动相进行洗脱,在主机转速800 r/min、体积流量1.5 mL/min、检测波长254 nm条件下进行分离制备。结果 从2.18 g荷叶提取物中一次分离得到N-去甲荷叶碱110 mg、O-去甲荷叶碱420 mg、荷叶碱310 mg和莲碱190 mg 4种生物碱,质量分数均大于98%;各化合物通过HPLC、MS和1H-NMR进行了化学结构鉴定。结论 pH区带逆流色谱法是一种快速高效的分离纯化荷叶生物碱的方法。
[Key word]
[Abstract]
Objective To explore the enhanced role of ultrasound on supercritical fluid extraction. Methods With stability parameters of supercritical fluid extraction of Magnoliae Officinalis Cortex, taking magnolol and honokiol contents and extraction rate as the reference indicators, the extraction effect between ultrasonic and supercritical fluid and ultrasound-enhanced supercritical fluid was compared. Rusults Ultrasound-enhanced supercritical fluid extraction is superior to the others. Conclusion Ultrasound could strengthen the supercritical fluid extraction of active ingredients from Magnoliae Officinalis Cortex.
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[基金项目]
国家科技支撑计划子课题(2006BAI09B07-04)