A triangulated approach combining high-resolution mass spectrometry, chromatographic fingerprints, and multivariate analysis for holistic quality assessment of Nardostachyos Radix et Rhizoma.

Nardostachyos Radix et Rhizoma (NR) is a traditional Asian herb with a long history of therapeutic use and has demonstrated pharmacological efficacy in digestive regulation, sedation, and spasmolysis. However, the chemical composition of NR is still unclear and the quality control remains inadequate. This study established a relatively complete chemical profile of NR through integrated liquid chromatograph-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) techniques. LC-MS analysis identified 96 non-volatile components, including 44 terpenoids and 16 organic acids, with fragmentation pathway elucidation for key compounds. GC-MS revealed 84 volatile compounds dominated by (+)-calarene. In addition, we further developed a multi-dimensional quality assessment system combining multi-wavelength high-performance liquid chromatography (HPLC) fingerprinting, GC-MS fingerprinting, and chemical pattern recognition for quality assessment of NR. This approach successfully mapped geographical variations across 9 production regions in China (Sichuan, Gansu, Qinghai, etc.), categorizing samples into 2 distinct groups. Seven key differential markers were identified for each analytical platform. Additionally, a multi-wavelength, multi-component quantitative analysis was performed to evaluate region-specific compositional differences. Taken together, the chemical constituents of NR were systematically identified and fingerprinting analysis coupled with chemical pattern recognition was successfully employed for evaluating the holistic quality, which will provide valuable insights and practical considerations for enhancing NR quality assessment.