Characterization and identification of chemical components in Si-Ni-San based on UPLC-Q-Orbitrap-MS, HS-SPME-GC-MS, and HS-GC-IMS techniques

Si-Ni-San (SNS) is a traditional Chinese medicine (TCM) formula known for its efficacy in dispelling evil spirits, relieving depression, dredging the liver and regulating the spleen. It is frequently utilized in clinical settings to address conditions like depression, anxiety, insomnia, liver fibrosis, and ulcerative colitis, among others. However, due to the complex composition of SNS, limited research has been conducted on its pharmacodynamic material basis. Therefore, this study aimed to qualitatively characterize the non-volatile components of SNS using ultraperformance liquid chromatography-quadrupole-orbitrap mass spectrometry (UPLC-Q-Orbitrap-MS), resulting in identification of 85 non-volatile components primarily composed of flavonoids. Additionally, volatile metabolites were elucidated through headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) and headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) techniques to comprehensively identify and characterize a total of 162 volatile components present in SNS. In addition, an optimized parallel reaction monitoring (PRM) method was developed using the UPLC-Q-Orbitrap MS platform to simultaneously quantify ten key components of SNS. In summary, this developed approach enables sensitive and precise qualitative and quantitative assessment of chemical components within SNS while providing a foundation for further basic research on these substances' quality assurance and formulation development.