高效液相色谱-四级杆-飞行时间串联质谱分析雪峰虫草化学成分  

Identification of chemical constituents in Ophiocordyceps xuefengensis sp. nov. by HPLC-Q-TOF-MS/MS

作　　者：张水寒[1,2] 蔡萍[1,2] 陈林[1,2] 梁雪娟[1,2] 秦优 朱如彩[1] 黄惠勇[1,2] 

机构地区：[1]湖南省中医药研究院中药研究所,湖南长沙410013 [2]湖南省2011数字中医药协同创新中心,湖南长沙410013

出　　处：《中草药》2015年第6期817-821,共5页Chinese Traditional and Herbal Drugs

基　　金：湖南省科技厅重大专项(2014FJ1007)

摘　　要：目的采用高效液相色谱-四级杆-飞行时间串联质谱法(HPLC-Q-TOF-MS/MS)对雪峰虫草醇提取物的主要化学成分进行分析鉴定。方法超声法制备雪峰虫草醇提取物,月旭AQ-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检测,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28个化合物的结构,其主要化学成分为甘露醇、腺苷、麦角甾醇、谷甾醇、氨基酸、脂肪酸、糖类等成分。结论 HPLC-Q-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雪峰虫草的主要成分进行定性分析,为寻找虫草中活性物质提供一种快速准确的分析方法。Objective Using the HPLC-Q-TOF-MS/MS to analyze and identify the main components in the ethanol extract of Ophiocordyceps xuefengensis sp. nov. Methods The ethanol extract ofO. xuefengensis sp. nov. was preparaed by using the ultrasonic methods, the main components in the extracts were separated by using the gradient elution method with RP-HPLC, Yuexu AQ-C18 column （250 mm × 4.6 mm, 5 μm）; The positive and negative electro spray ionization （ESI） source was used for determine the chromatographic effluent, the main chromatographic peaks are assigned by Q-TOF. Results Based on the standards of MS/MS and compared with the reference results, 28 compounds, containing maunitol, adenosine, ergosterol, sitosterol, amino acid, fatty acid, and sugar, were identified. Conclusion HPLC-ESI-TOF-MS/MS method can qualitatively analyze the main components in O. xuefengensis sp. nov. from the retention time, UV spectrum, precious relative molecular weight, formula, secondary fragment ions, and so on. It is an effective and fast analysis method for determining the active compounds in O. xuefengensis sp. nov.

关 键 词：雪峰虫草 高效液相色谱-四级杆-飞行时间串联质谱 定性分析 腺苷 麦角甾醇 氨基酸 

分 类 号：R284.1[医药卫生—中药学]