【目的】利用超高效液相色谱与串联四级杆飞行时间质谱仪联用技术(ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry,UPLC-Q-TOF-MS/MS)结合质谱裂解规律分析,靶向分离Alternaria pa...【目的】利用超高效液相色谱与串联四级杆飞行时间质谱仪联用技术(ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry,UPLC-Q-TOF-MS/MS)结合质谱裂解规律分析,靶向分离Alternaria panax发酵液粗提物中次生代谢产物。【方法】用马铃薯葡萄糖(potato dextrose broth,PDB)培养基液体发酵A.panax 14 d,将滤液用乙酸乙酯萃取后减压浓缩得粗提物;基于UPLC-Q-TOF-MS/MS方法(高分辨质谱、分子式与碎片峰等)分析粗提物化学成分及质谱裂解规律;采用半制备高效液相色谱(high-performance liquid chromatography,HPLC)方法进一步分离纯化;结合核磁共振波谱(nuclear magnetic resonance,NMR)和质谱(mass spectrometry,MS)等谱学技术以及与文献数据对照确定化合物结构。【结果】利用UPLC-Q-TOF-MS/MS技术分析出A.panax发酵液中存在9个二酮哌嗪类化合物(1-9),并分析其质谱裂解规律;为验证结构推测的准确性,靶向分离鉴定了化合物1-3,结合高分辨质谱数据,靶向分离得到的化合物结构与质谱分析结构一致。【结论】UPLC-Q-TOF-MS/MS技术结合质谱裂解规律能够快速、高效地完成样品中目标成分的分析,并可以指导化合物的靶向分离。展开更多
Twelve indolyl diketopiperazines 1-12 were isolated from the mycelia culture of Aspergillus penicilliodes Speg.,a dominant microorganism from the post fermentation process of ripe Pu-er tea.Their structures were eluci...Twelve indolyl diketopiperazines 1-12 were isolated from the mycelia culture of Aspergillus penicilliodes Speg.,a dominant microorganism from the post fermentation process of ripe Pu-er tea.Their structures were elucidated by extensive spectroscopic methods.Among them,trypostatins C(1)and D(2)featuring with a rare methyl vinyl ketone side chain at C-2 are new compounds,while 3 and 4 were obtained for the first time from nature source.The isolates 3-12 did not show obvious cytotoxicities against five human cancer cell lines at a concentration of 40μM.展开更多
基金supported by the National Natural Science Foundation of China(No.21672223).
文摘Twelve indolyl diketopiperazines 1-12 were isolated from the mycelia culture of Aspergillus penicilliodes Speg.,a dominant microorganism from the post fermentation process of ripe Pu-er tea.Their structures were elucidated by extensive spectroscopic methods.Among them,trypostatins C(1)and D(2)featuring with a rare methyl vinyl ketone side chain at C-2 are new compounds,while 3 and 4 were obtained for the first time from nature source.The isolates 3-12 did not show obvious cytotoxicities against five human cancer cell lines at a concentration of 40μM.
