Key Laboratory of Mountain Ecological Restoration and Bioresource Utilization, Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu 610041, China.
J Pharm Biomed Anal. 2011 Dec 15;56(5):916-27. doi: 10.1016/j.jpba.2011.07.045. Epub 2011 Aug 4.
An ultra performance liquid chromatography (UPLC) coupled with quadrupole time-of-flight mass spectrometry (QTOF-MS) procedure is designed for the first simultaneous analysis of nortriterpenoids and lignans in Schisandra samples. The method consists of three individual mass spectrometric experiments, including the full scan MS, MS/MS experiment and in-source collision induced dissociation (CID) MS/MS, which enable the identification of diagnostic fragmentation pathways of nortriterpenoids and lignans. As such, a total of 6 nortriterpenoids and 10 lignans were unequivocally identified, and one nortriterpenoid and 20 lignans were tentatively identified from different Schisandra samples within 12.5 min. In addition, 6 nortriterpenoids and 10 lignans were quantified in 48 samples of S. chinensis and S. sphenanthera using an extract ion chromatogram (XIC) of the full scan MS experiment. Dataset obtained from UPLC-MS was processed with principal component analysis (PCA) and orthogonal partial least squared discriminant analysis (OPLS-DA) to compare the difference between the two Schisandra species.
建立了一种超高效液相色谱-四极杆飞行时间串联质谱(UPLC-QTOF-MS)方法，用于首次同时分析五味子样品中的三萜和木脂素。该方法包括三个独立的质谱实验，包括全扫描 MS、MS/MS 实验和源内碰撞诱导解离( CID ) MS/MS，这些实验可识别三萜和木脂素的特征碎片途径。因此，从不同的五味子样品中总共鉴定出 6 种三萜和 10 种木脂素，其中 1 种三萜和 20 种木脂素为初步鉴定。此外，采用全扫描 MS 实验的提取离子色谱图(XIC)，对 48 份中华五味子和华中五味子样品中的 6 种三萜和 10 种木脂素进行了定量分析。利用主成分分析(PCA)和正交偏最小二乘判别分析(OPLS-DA)对两种五味子的差异进行了比较。
