Ligustri Lucidi Fructus (LLF), the fruit of Ligustrum lucidum Ait. (Oleaceae), has been used as a common herbal medicine in clinical practice in China for nearly 2000 years. In most cases, LLF is prescribed in decoctions in the form of processed products rather than crude drugs. In this study, an ultra-high performance liquid chromatography coupled with electrospray ionization-quadrupole-time of flight-mass spectrometry (UHPLC-ESI-Q-TOF-MS) method was established for rapid separation and identification of multiple constituents in the 80% methanol extract of processed-LLF. A total of 50 compounds (one phenylethanoid, seven phenylethanoid glycosides, seven flavonoids, 25 iridoids, nine triterpenoids and one cyclohexanecarboxylic acid) were either unambiguously identified or tentatively characterized with the aid of authentic standards or published data. Luteolin-7-O-rutinoside, oleoside and secologanoside were detected in LLF for the first time. This study enriches the chemical profiling of processed-LLF and could provide valuable information for the quality control and further investigation of processed-LLF and crude LLF.

Amentoflavone is one of the important bioactive flavonoids in the ethylacetate extract of "Cebaiye", which is a blood cooling and hematostatic herb in traditional Chinese medicine. The previous work in our group has demonstrated that the ethylacetate extract of Cebaiye has a notable antagonistic effect on the injury induced by lipopolysaccharide (LPS) to human umbilical vein endothelial cells (HUVECs). The present investigation was designed to assess the effects and possible mechanism of cytoprotection of amentoflavone via metabolomics. Ultra-performance liquid chromatography/quadrupole time of flight-mass spectrometry (UPLC/QTOF-MS) coupled with multivariate data analysis was used to characterize the variations in the metabolites of HUVECs in response to exposure to LPS and amentoflavone treatment. Seven putative metabolites (glycine, argininosuccinic acid, putrescine, ornithine, spermidine, 5-oxoproline and dihydrouracil) were discovered in cells incubated with LPS and/or amentoflavone. Functional pathway analysis uncovered that the changes of these metabolites related to various significant metabolic pathways (glutathione metabolism, arginine and proline metabolism, β-alanine metabolism and glycine, serine and threonine metabolism), which may explain the potential cytoprotection function of amentoflavone. These findings also demonstrate that cellular metabolomics through UPLC/QTOF-MS is a powerful tool for detecting variations in a range of intracellular compounds upon toxin and/or drug exposure.

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An ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry method has been established to evaluate the variations of multiple components of Chinese herbal preparations, Jiao-ai decoction and Si-wu decoction, through the simultaneous determination of eight major active compounds with a huge difference in the level of content. Chromatographic separation was achieved on a Waters Acquity UPLC BEH C18 column (2.1 × 100 mm, 1.7 μm) with a mobile phase consisting of acetonitrile (0.1% formic acid) and water (0.1% formic acid) under gradient elution. A triple quadrupole tandem mass spectrometer was operated in positive and negative ionization modes, respectively, with multiple reaction monitoring for the detection of the eight compounds. All calibration curves showed excellent linear regressions (r > 0.99) within the test range. The precision, repeatability, and stability of the eight compounds were below 5.0% in terms of relative standard deviation. The recoveries were 97.0-102.4% with a relative standard deviation of 1.21-3.65% for all samples. In conclusion, a rapid, sensitive, precise, accurate, and reliable method has been developed for the simultaneous detection of eight active compounds in the pharmaceutical samples of Jiao-ai decoction and Si-wu decoction, which can be applied for the multicomponent comparison and further quality control.