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60mg茄尼醇粗提物中分离得到了5mg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。
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 I. 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.
出处
《色谱》
CAS
CSCD
北大核心
2007年第4期528-531,共4页
Chinese Journal of Chromatography
关键词
高速逆流色谱
大气压化学电离质谱
茄尼醇
土豆叶
制备分离
high-speed counter-current chromatography （ HSCCC ）
atmosphericchemical ionization mass spectrometry （APCI-MS）
solanesol
potatopreparative isolationpressure leaves
