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.
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.
参考文献
| [1] | Chen L,Deng L J,Chen P.Chinese Journal of Chromatography (陈理,邓丽杰,陈平.色谱),2006,24(6):570 |
| [2] | Ito Y.J Chromatogr A,2005,1065:145 |
| [3] | Zhou T T,Fan G R.Journal of China Pharmaceutical University (周婷婷,范国荣.中国药科大学学报),2007,38(5):391 |
| [4] | Qi Y Y,Meng Z L,Liu R M.Chemical Analysis and Meterage (齐元英,孟兆玲,柳仁民.化学分析计量),2006,15(6):95 |
| [5] | Friesen J B,Pauli G F.J Chromatogr A,2007,1151:51 |
| [6] | Yao S,Luo J G,Huang X F,et al.J Chromatogr B,2008,864:69 |
| [7] | Cao X L.World Science and Technology:Modernization of Traditional Chinese Medicine and Materia Medica (曹学丽.世界科学技术:中医药现代化),2007,9(1):54 |
| [8] | Dai R Q,Li X M,Shao A J,et al.Mycosystema (戴如琴,李晓明,邵爱娟,等.菌物学报),2008,27(5):642 |
| [9] | Jiang Y,Yao Y J.Mycosystema (蒋毅,姚一建.菌物系统),2003,22(1):161 |
| [10] | Luan L,Wang G L,Yu J P,et al.Chinese Traditional and Herbal Drugs (栾兰,王钢力,郁建平,等.中草药),2007,38(6):825 |
| [11] | Deng Y Q,Wang J,Yu L.Journal of Microbiology (邓玉清,王纪,虞龙.微生物学杂志),2001,21(3):54 |
| [12] | Xu X Q,Hong W R,Chen D J.Chinese Journal of Antibiotics (许向前,洪文荣,陈代杰.中国抗生素杂志),2006,31(6):379 |
| [13] | Yang R Y,Li C Y,Lin Y C,et al.Journal of Chinese Medicinal Materials (杨瑞云,李春远,林永成,等.中药材),2006,29(9):908 |
| [14] | Yao S,Liu R M,Huang X F,et al.Chinese Journal of Natural Medicines (姚舜,柳仁民,黄雪峰,等.中国天然药物),2008,6(1):13 |
| [15] | Cao X L.Isolation Technology and Application of High-Speed Counter Current Chromatography.Beijing:Chemical Industry Press (曹学丽.高速逆流色谱分离技术及应用.北京:化学工业出版社),2004:44 |
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