色谱

色谱

• 研究论文 • 上一篇    下一篇

高速逆流色谱法从蝙蝠蛾拟青霉中快速分离制备麦角甾醇纯品

章能胜, 王金彬, 汪小艳, 王小董, 胡丰林*   

  1. 安徽农业大学, 安徽省微生物防治重点实验室, 安徽 合肥 230036
  • 收稿日期:2009-05-20 修回日期:2009-07-20 出版日期:2010-01-28 发布日期:1981-09-25
  • 通讯作者: 胡丰林

Preparative isolation and purification of ergosterol from a strain of Paecilomyces hepialid by high-speed counter-current chromatography

ZHANG Nengsheng, WANG Jinbin, WANG Xiaoyan, WANG Xiaodong, HU Fenglin*   

  1. Anhui Provincial Key Laboratory of Microbial Pest Control, Anhui Agricultural University, Hefei 230036, China
  • Received:2009-05-20 Revised:2009-07-20 Online:2010-01-28 Published:1981-09-25
  • Contact: HU Fenglin

PDF

563

摘要： 建立了用高速逆流色谱从蝙蝠蛾拟青霉中高效、快速分离制备高纯度麦角甾醇的方法。将蝙蝠蛾拟青霉的乙酸乙酯提取物直接进行高速逆流色谱分离,考察了不同溶剂系统的分离效果。结果表明,最佳的溶剂系统为正己烷-乙酸乙酯-甲醇-水(体积比为6:1.7:6:0.3),以上相为固定相,下相为流动相,转速为850 r/min,流速为2 mL/min,检测波长为280 nm。制备所得的麦角甾醇经紫外光谱(UV)和高分辨质谱(HRMS)鉴定及与标准品对照定性;纯度经高效液相色谱(HPLC)分析为99.2%(峰面积归一化法)。该方法制备麦角甾醇简便、快速,所得产物的纯度高,适合于麦角甾醇对照品的制备。

关键词: 蝙蝠蛾拟青霉 , 高速逆流色谱, 麦角甾醇, 制备

Abstract: To develop an effective and rapid method for the preparation of ergosterol from a strain of Paecilomyces hepialid, the ethyl acetate extract of the mycelia was injected into a high-speed counter-current chromatograph (HSCCC) directly, and eluted with different solvent systems. The result showed that the solvent system composed of n-hexane-ethyl acetate-methanol-water (6:1.7:6:0.3, v/v/v/v) was the best. The lower phase was used as the mobile phase and performed at a flow rate of 2 mL/min, while the apparatus rotated at 850 r/min, and detected at 280 nm. The prepared ergosterol was identified with ultraviolet detection (UV), high resolution mass spectrometer (HRMS) and standard, and its purity was 99.2% analyzed by high performance liquid chromatography. The established method is relatively simple, fast, and suitable for the large-scale isolation and separation of ergosterol.

Key words: ergosterol, Paecilomyces hepialid , preparation, high-speed counter-current chromatography (HSCCC)