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  被引量:12

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

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作  者:章能胜[1] 王金彬[1] 汪小艳[1] 王小董[1] 胡丰林[1] 

机构地区:[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

出  处:《色谱》2010年第1期68-72,共5页Chinese Journal of Chromatography

基  金:国家自然科学基金项目(No.30871676);安徽省高校自然科学研究重点项目(DT200708)

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850r/min,流速为2mL/min,检测波长为280nm。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。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.

关 键 词:高速逆流色谱 制备 麦角甾醇 蝙蝠蛾拟青霉 

分 类 号:O658[理学—分析化学]

 

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