CAJ | 학술논문

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.
건립료용고속역류색보종편복아의청매중고효、쾌속분리제비고순도맥각치순적방법.장편복아의청매적을산을지제취물직접진행고속역류색보분리,고찰료불동용제계통적분리효과.결과표명,최가적용제계통위정기완-을산을지-갑순-수(체적비위6∶1.7∶6∶0.3),이상상위고정상,하상위류동상,전속위850 r/min,류속위2 mL/min,검측파장위280 nm.제비소득적맥각치순경자외광보(UV)화고분변질보(HRMS)감정급여표준품대조정성;순도경고효액상색보(HPLC)분석위99.2%(봉면적귀일화법).해방법제비맥각치순간편、쾌속,소득산물적순도고,괄합우맥각치순대조품적제비.
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.