摘要
采用高速逆流色谱法分离纯化库拉索芦荟中的2’-对香豆酰芦荟宁。以正己烷-乙酸乙酯-丙酮-水(1∶5∶1∶5,V/V/V/V)为溶剂体系,上相为固定相,下相为流动相,线圈转速为860 r/min,流速为2 mL/min,紫外检测波长为300 nm,一次进样85 min内从487.5 mg库拉索芦荟丙酮提取物中分离得到19.5 mg单体组分,经高效液相色谱分析,测定纯度为95.6%(峰面积百分比),通过质谱、红外、紫外和核磁技术进行结构鉴定,确定组分为2’-对香豆酰芦荟宁。该法具有操作简便、速度快、样品制备量大、节省溶剂及回收率高等优点,可为芦荟宁类化合物的分离提供高效、稳定及可靠的方法。
Aloenin-2＇-p-coumaroyl ester was separated and purified from Aloe barbadensis Mill by one step of high-speed counter-current chromatography. The separation was performed with an optimized two-phase solvent system composed of hexane-ethyl acetate- acetone-water （1：5：1：5, V/V/V/V）, using the lower phase as the mobile phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase, and UV detection wavelength was 860 rpm, 2.0 mL/min and 300 nm, respectively. In a one-step operation within 85 min, 19.5 mg of aloenin-2＇-p-coumaroyl ester could be obtained from 487.5 mg of dried acetone extract at purities of 95.6%, as determined by HPLC using area normalization method. The structure of the compound was identified by high resolution mass spectroscopy （HRMS）, UV, IR and NMR. h is simple, fast and it eliminates the irreversible loss of samples, resulting in a higher recovery and larger scale of products than conventional techniques. This experiment gives an efficient, stable and reliable technique to prepare high pure aloenin nature products.
出处
《热带作物学报》
CSCD
北大核心
2014年第8期1632-1637,共6页
Chinese Journal of Tropical Crops
基金
"十二五"农村领域国家科技计划课题"区域特产资源生态高值加工质量安全控制关键技术研究"(No.2012BAD36B02)
关键词
高速逆流色谱
库拉索芦荟
2’-对香豆酰芦荟宁
分离纯化
High-speed counter-current chromatography
Aloe barbadensis Mill
Aloenin-2＇-p-coumaroyl ester
Isolation and purification
