高效液相色谱-电喷雾-飞行时间串联质谱分析泽兰水提物  

Identification of compounds in aqueous extract from aerial parts of Lycopus lucidus by HPLC-ESI-TOF-MS/MS

作　　者：黄晶晶[1] 李倩[1] 高小康[1] 赵新锋[1] 王世祥[1] 郑晓晖[1,2] 

机构地区：[1]西北大学生命科学学院,陕西西安710069 [2]西北大学与深圳清华大学研究院共建"创新中药及天然药物研究"联合实验室,广东深圳518057

出　　处：《中草药》2013年第16期2218-2222,共5页Chinese Traditional and Herbal Drugs

基　　金：国家自然科学基金资助项目(21005060);高等学校博士学科点专项科研基金(20106101110001)

摘　　要：目的采用高效液相色谱-电喷雾-飞行时间串联质谱法(HPLC-ESI-TOF-MS/MS)对泽兰水提物的主要成分进行分析鉴定。方法超声法制备泽兰水提物,TC-C18(250 mm×4.6 mm,5μm)反相HPLC梯度洗脱法分离各主要成分;电喷雾电离源正离子模式和负离子模式对色谱流出物进行离子化,四级杆飞行时间串联质谱法对各主要色谱峰进行归属。结果通过二级高分辨质谱分析结合对照品数据及相关文献共鉴定22个化合物的结构,其主要结构类型为氨基酸类、酚酸类、萜类、黄酮及黄酮苷类、甾醇类和脂肪酸类。结论 HPLC-ESI-TOF-MS/MS可从保留时间、紫外吸收光谱、精确相对分子质量、分子式和二级结构碎片等方面对泽兰的主要成分进行定性分析,为中药药效物质基础研究提供一种快速准确的分析方法。Objective To identify the main active compounds in the aqueous extract from the aerial parts of Lycopus lucidus by high performance liquid chromatography （HPLC）-electrospray （ESI）-time of flight tandem mass spectrometry （TOF-MS/MS）. Methods The aqueous extract from the aerial parts of L. lucidus was prepared using ultrasonic method; Chromatographic separation of the main active compounds was performed on a TC-C18 （250 mm × 4.6 mm, 5 μm） reverse phase column through gradient elution; All the compounds eluted from the column were detected under both positive and negative ionization modes. Each chromatographic peak was analyzed by quadrupole tandem mass spectrometry coupled with TOF. Results Twenty two compounds were identified through the analysis of tandem mass spectrum and the information from reference substances, including amino acids, phenolic acids, terpenoids, flavonoids and flavonoid glycosides, sterols, and fatty acid. Conclusion HPLC-ESI-TOF-MS/MS is capable of analyzing the main compounds in the aerial parts of L. lucidus using retention time, ultraviolet spectrum, current molecular weight, formula, and fragmenting information of daughter ions. It will probably become a reliable alternative for the rapid analyzing substantial foundation of Chinese materia medica.

关 键 词：泽兰 高效液相色谱-电喷雾-飞行时间串联质谱 二级高分辨质谱 药效物质基础 定性分析 

分 类 号：R284.1[医药卫生—中药学]