Integrated Liquid Chromatography-Tandem Mass Spectrometry and Headspace Solid-Phase Microextraction With Gas Chromatography-Mass Spectrometry-based Profiling Reveals Developmental Metabolic Dynamics of Ligusticum striatum DC.

Ligusticum striatum DC. (Ligusticum chuanxiong Hort. or Ligusticum wallichii) is a traditional medicinal herb in East Asia used for cardiovascular, neurological, and inflammatory disorders, but developmental phytochemical changes remain unclear. Here, targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) and untargeted headspace solid-phase microextraction with gas chromatography-MS were applied to examine five bioactive compounds and volatile organic compounds (VOCs) in aerial and root tissues across seven growth periods. Five compounds, including ferulic acid, icariside F2, ligusticoside A, N-3-(3-methoxy-4-hydroxyphenyl) allyl pipecolic acid, and ligustiphenol, were quantified with excellent linearity, sensitivity, precision, and accuracy. VOC profiling identified 33 and 32 compounds in aerial parts and roots, respectively, showing clear period- and tissue-specific differences. Chemometrics analysis revealed distinct clustering by growth stage, indicating dynamic metabolic shifts. Overall, roots served as reservoirs of phenolic acids, while aerial parts were enriched in phthalides and sesquiterpenes. These findings provide a basis for harvest optimization, quality control, and standardization of L. striatum, while novel compounds in Vietnamese herbal medicines expand its phytochemical diversity and pharmacological potential.