Zhang Xiaozhe, Liang Xinmiao, Xiao Hongbin, Xu Qing
Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian, China.
J Am Soc Mass Spectrom. 2004 Feb;15(2):180-7. doi: 10.1016/j.jasms.2003.09.014.
The applicability of on-line coupling of reversed-phase high-performance liquid chromatography to atmospheric pressure ionization tandem mass spectrometry for the separation and characterization of hop acids mixture from the crude extract of Humulus lupulus was investigated. The solvent system consisting of acetonitrile-aqueous formic acid was used to give proper separation of the six main hop bitter acids within 30 min. Further structural information about the components was acquired by collision-induced dissociation (CID). On the basis of analyses of the fragmentation patterns of the major alpha- and beta-bitter acids respectively, identification of the minor ones was performed using selected reaction monitoring (SRM) with a group of qualitatively relevant selected precursor-product ion transitions for each bitter acid in a single high performance liquid chromatography (HPLC) run. Using this technique, six minor hop acids, including "adprelupulone" observed for the first time in natural resources, were detected along with the six major acids. This hyphenated techniques provides potency for rapid qualitative determination of analogs and homologs in mixtures.
研究了反相高效液相色谱与大气压电离串联质谱在线联用技术用于分离和表征啤酒花粗提物中啤酒花酸混合物的适用性。采用由乙腈 - 甲酸水溶液组成的溶剂系统，在30分钟内对六种主要啤酒花苦味酸进行了适当分离。通过碰撞诱导解离（CID）获得了有关组分的进一步结构信息。在分别分析主要α-和β-苦味酸的碎裂模式的基础上，在一次高效液相色谱（HPLC）运行中，针对每种苦味酸，使用一组定性相关选择的前体 - 产物离子跃迁，通过选择反应监测（SRM）对次要苦味酸进行鉴定。使用该技术，除了六种主要酸之外，还检测到六种次要啤酒花酸，包括首次在自然资源中观察到的“前异律草酮”。这种联用技术为混合物中类似物和同系物的快速定性测定提供了能力。
