Shang, Z. Xu, L. Xiao, Y. Du, W. An, R. Ye, M. Qiao, X. text xx 9999 monographic und

electronic

Although ultraviolet detector or mass spectrometer could be coupled with two-dimensional liquid chromatography (2DLC)to analyze complex constituents, full detection and identification of the compounds are difficult. Suffering from biased UV detection and insufficient MS data interpretation, a number of minor compounds are neglected though they are separated. In this study, we report a global chemical profiling strategy using comprehensive 2DLC coupled with dual-MS platforms, including Orbitrap-MS and QqQ-MS. It was exemplified by an 11-herb Chinese medicine formula Xiaoer-Feire-Kechuan (XFK). Firstly, constituents in XFK were separated on a CSH C18 × Phenyl-Hexyl 2DLC system with a practical peak capacity of 990.5 and an orthogonality of 90.3 percent. Secondly, untargeted mass spectral data was collected using dd-MS2 scan on an Orbitrap-MS. In total 542 peaks were detected, which was 4 times of that detected by 2DLC/UV (131 peaks). A total of 108 compounds were tentatively identified. Thirdly, targeted mass spectral data was collected for 8 characteristic substructures using neutral loss and precursor ion (NL/PRE)scan on a QqQ-MS. Extracted ion chromatogram was used to recognize minor constituents. An additional of 151 compounds were detected. Our study indicated that comprehensive 2DLC coupled with dd-MS2 and NL/PRE-MS is a powerful technique for the global profiling of multi-component systems. CHINESE MEDICINE FORMULA MULTI-COMPONENT SYSTEM NL/PRE SCAN TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY (2DLC) 2DLC/MS XIAOER-FEIRE-KECHUAN (XFK) https://drive.google.com/file/d/1hnUXLn8Sfq_fj18yCznF2DDyaT2V9zNQ/view?usp=drivesdk https://drive.google.com/file/d/1hnUXLn8Sfq_fj18yCznF2DDyaT2V9zNQ/view?usp=drivesdk 250602 20260521091635.0