色谱

色谱

• 研究论文 • 上一篇    下一篇

土豆叶中茄尼醇的高速逆流色谱法分离纯化及质谱解析

胡江涌,梁勇,谢亚,黄肇锋,钟汉佐

  

  1. School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
  • 收稿日期:2007-01-05 修回日期:2007-03-21 出版日期:2007-07-30 发布日期:1985-06-25
  • 通讯作者: 梁勇

Isolation and Purification of Solanesol from Potato Leaves
by High-Speed Counter-Current Chromatography and
Identification by Atmospheric Pressure Chemical
Ionization Mass Spectrometry

HU Jiangyong, LIANG Yong, XIE Ya, HUANG Zhaofeng, ZHONG Hanzuo   

  1. School of Chemistry and Environment, South China Normal University, Guangzhou 510006, China
  • Received:2007-01-05 Revised:2007-03-21 Online:2007-07-30 Published:1985-06-25

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摘要：

采用超微回流提取方法提取土豆叶中的茄尼醇,用高速逆流色谱(HSCCC)对粗提物中的茄尼醇进行分离纯化。以正己烷-甲醇(体积比为10∶7)作为两相溶剂系统,以其下相为流动相，上相为固定相，经过一步HSCCC从60 mg茄尼醇粗提物中分离得到了5 mg 纯度为98.7%的茄尼醇；对分离得到的茄尼醇进行大气压化学电离质谱解析,研究了茄尼醇的大气压化学电离质谱的一级电离规律和二级质谱裂解规律。

关键词: 大气压化学电离质谱, 高速逆流色谱, 茄尼醇, 土豆叶, 制备分离

Abstract:

Preparative high-speed counter-current chromatography (HSCCC) was used for the isolation and purification of solanesol from potato leaves. Experimental conditions of the extraction of solanesol from potato leaves have been optimized. An ultrafine extraction method was applied in this study. The efficiency using an ultrafine extraction was found to be improved in the investigation, the yields of solanesol by different extraction methods were 0.083% by ultrafine extraction and 0.050% by ultrasonic extraction. Using n-hexane-methanol (10∶7, v/v) as the two-phase solvent system, preparative HSCCC was successfully performed with the yield of 5 mg solanesol at 98.7% of purity from 60 mg of crude extract in the one-step separation. The mobile phase was the lower phase and operated at a flow rate of 1.5 mL/min, while the apparatus rotated at 800 r/min. The solanesol was identified by the atmospheric pressure chemical ionization mass spectrometry （APCI-MS）. The ionization and cleavage mechanisms of solanesol in APCI-MS and APCI-MS/MS are discussed.

Key words: atmospheric pressure chemical ionization mass spectrometry （APCI-MS）, potato leaves, preparative isolation , solanesol, high-speed counter-current chromatography （HSCCC）