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Systematic Profiling of the Multicomponents and Authentication of Erzhi Pill by UHPLC/Q-Orbitrap-MS Oriented Rapid Polarity-Switching Data-Dependent Acquisition and Selective Monitoring of the Chemical Markers Deduced from Fingerprint Analysis

by Li Jia 1,2,†, Lingling Fu 1,2,†, Xiaoyan Wang 1,2, Wenzhi Yang 1,2,*, Hongda Wang 1,2, Tiantian Zuo 1,2, Chunxia Zhang 1,2, Ying Hu 1,2, Xiumei Gao 1 and Lifeng Han 1,2,*
1
Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, 312 Anshanxi Road, Tianjin 300193, China
2
Tianjin Key Laboratory of TCM Chemistry and Analysis, Tianjin University of Traditional Chinese Medicine, 312 Anshanxi Road, Tianjin 300193, China
*
Authors to whom correspondence should be addressed.
These two authors contributed equally to this work.
Molecules 2018, 23(12), 3143; https://doi.org/10.3390/molecules23123143
Received: 8 November 2018 / Revised: 28 November 2018 / Accepted: 28 November 2018 / Published: 30 November 2018
The analytical platform UHPLC/Q-Orbitrap-MS offers a solution to quality investigation of TCM with high definiteness. Using Erzhi Pill (EZP) as a case, we developed UHPLC/Q-Orbitrap-MS based approaches to achieve systematic multicomponent identification and rapid authentication. Comprehensive multicomponent characterization of EZP was performed by negative/positive switching data-dependent high-energy collision-induced dissociation-MS2 (HCD-MS2) after 25 min chromatographic separation. By reference compounds comparison, elemental composition analysis, fragmentation pathways interpretation, and retrieval of an in-house library, 366 compounds were separated and detected from EZP, and 96 thereof were structurally characterized. The fingerprints of two component drugs (Ligustri Lucidi Fructus, LLF; Ecliptae Herba, EH) for EZP were analyzed under the same LC-MS condition by full scan in negative mode. In combination with currently available pharmacological reports, eight compounds were deduced as the ‘identity markers’ of EZP. Selective ion monitoring (SIM) of eight marker compounds was conducted to authenticate six batches of EZP samples. Both LLF and EH could be detected from all EZP samples by analyzing the SIM spectra, which could indicate their authenticity. Conclusively, UHPLC/Q-Orbitrap-MS by rapid polarity switching could greatly expand the potency of untargeted profiling with high efficiency, and SIM of multiple chemical markers rendered a practical approach enabling the authentication of TCM formulae. View Full-Text
Keywords: Erzhi Pill; UHPLC/Q-Orbitrap-MS; polarity-switching data-dependent acquisition; identity marker; authentication; selective ion monitoring Erzhi Pill; UHPLC/Q-Orbitrap-MS; polarity-switching data-dependent acquisition; identity marker; authentication; selective ion monitoring
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Jia, L.; Fu, L.; Wang, X.; Yang, W.; Wang, H.; Zuo, T.; Zhang, C.; Hu, Y.; Gao, X.; Han, L. Systematic Profiling of the Multicomponents and Authentication of Erzhi Pill by UHPLC/Q-Orbitrap-MS Oriented Rapid Polarity-Switching Data-Dependent Acquisition and Selective Monitoring of the Chemical Markers Deduced from Fingerprint Analysis. Molecules 2018, 23, 3143.

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