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高速逆流色谱法制备分离库拉索芦荟中的2’-对香豆酰芦荟宁

Isolation and Purification of Aloenin-2’-p-coumaroyl Ester from Aloe barbadensis Mill by High-speed Counter-current Chromatography

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【作者】 吴小芳; 万金志; 钟佳胜; 罗金辉; 黎舒怀; 张群;

【Author】 WU Xiaofang;WAN Jinzhi;ZHONG Jiasheng;LUO Jinhui;LI Shuhuai;ZHANG Qun;Analysis and Testing Center, Chinese Academy of Tropical Agricultural Sciences;Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables;School of Pharmaceutical Sciences, Sun Yat-Sen University;

【机构】 中国热带农业科学院分析测试中心; 海南省热带果蔬产品质量安全重点实验室; 中山大学药学院药物分析实验室;

【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。

【Abstract】 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. It 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.

【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)
  • 【文献出处】 热带作物学报 ,Chinese Journal of Tropical Crops , 编辑部邮箱 ,2014年08期
  • 【分类号】S567.239
  • 【被引频次】1
  • 【下载频次】104
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