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半制备高效液相色谱法分离制备香鳞毛蕨中间苯三酚类衍生物 |
Isolation and Preparation of Phloroglucinol Derivatives from Dryopteris Fragrans by Semi preparation HPLC |
投稿时间:2014-10-23 修订日期:2014-12-28 |
DOI: |
中文关键词: 半制备液相色谱法 香鳞毛蕨 间苯三酚类衍生物 绵马素BB 绵马素PB |
英文关键词:Semi preparation HPLC Dryopteris fragrans Phloroglucinol derivatives Aspidin BB Aspidin PB |
基金项目:国家自然科学基金项目(编号:81202885);科技部“十二五”重大新药创制项目(编号:2011zx09102-007-03);广东省科技计划项目(编号:2010B0307000444);广州市科技计划项目(编号:12A062131631) |
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中文摘要: |
摘 要 目的: 采用半制备液相色谱法从香鳞毛蕨中分离制备间苯三酚类衍生物的对照品。 方法: 用石油醚回流提取香鳞毛蕨,提取液浓缩后经硅胶柱色谱分离,再用半制备高效液相制备,以纯乙腈为流动相进行等度洗脱(3 ml· min-1),进样量为0.5 ml,得到2个间苯三酚类衍生物。结果:2个化合物结构分别为绵马素BB和绵马素PB,经超高效液相色谱法(UPLC)测定纯度,分别为绵马素BB(98.81%)、绵马素PB(98.57%)。结论: 该方法制备的绵马素BB和绵马素PB纯度较高都在98%以上,简单,快速,可用于对照品的制备。 |
英文摘要: |
ABSTRACT Objective: To isolate and prepare the reference substances of phloroglucinol derivatives from Dryopteris fragrans by semi-preparation HPLC. Methods: After reflux extraction of Dryopteris fragrans with petroleum ether, the extracting solution was concentrated and separated by silica gel column chromatography, and then isolated by semi-preparation HPLC. The isocratic elution was carried out using acetonitrile as the mobile phase at 3.0 ml·min-1 and the injection volume was 0.5 ml. Two phloroglucinol derivatives were isolated.Results: The chemical structure of the two phloroglucinol derivatives respectively was aspidin BB with the purity of 98.81% and aspidin PB with the purity of 98.57% by ultra high performance liquid chromatography. Conclusion:The isolation of aspidin BB and aspidin PB by semi preparation HPLC is simple and fast with the purity over 98%, which can be used to prepare the reference substances. |
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