title: Bioactivity-based ultra-performance liquid chromatography-coupled quadrupole time-of-flight mass spectrometry for NF-κB inhibitors identification in Chinese Medicinal Preparation Bufei Granule.
abstract: Traditional Chinese medicine (TCM) preparations have become effective treatments for many diseases. However, their active ingredients are still uncertain and difficult to identify. In this study, we propose a strategy that integrates ultra-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS) and bioactive (NF-κB inhibitor) luciferase reporter assay systems for the rapid determination of various anti-inflammatory compounds of TCM preparations. In this way, Bufei Granule (BFG), a TCM preparation used for the clinical therapy of asthma, was analyzed by the two ways of component identification and activity detection. Potential anti-inflammatory constituents were screened by NF-κB activity assay systems and simultaneously identified according to the mass spectrometry data. Three structural types of NF-κB inhibitors (caffeic acid derivatives, flavonoids and Pentacyclic triterpenes) were characterized. Further cytokine detection confirmed the anti-inflammatory effects of the potential NF-κB inhibitors. Compared with conventional chromatographic separation and inhibitory activity detection, integrating UPLC/Q-TOF-MS identification and virtual validation was more convenient and more reliable. This strategy clearly demonstrates that MS data-based fingerprinting is a meaningful tool not only in identifying constituents in complex matrix but also in directly screening for powerful trace ingredients in TCM preparations. Copyright © 2016 John Wiley & Sons, Ltd.
authors.affiliation: State Key Laboratory of Medicinal Chemical Biology and College of Pharmacy, Nankai University, Tianjin, 300071, People's Republic of China.
authors.forename: Cui
authors.initials: C
authors.lastname: Qingxin
authors.affiliation: Second Affiliated Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin, 300071, People's Republic of China.|Institute of Basic Research in Clinical Medicine, China Academy of Chinese Medical Sciences, Beijing, 100700, People's Republic of China.
authors.forename: Fu
authors.initials: F
authors.lastname: Min
authors.affiliation: State Key Laboratory of Medicinal Chemical Biology and College of Pharmacy, Nankai University, Tianjin, 300071, People's Republic of China.
authors.forename: Zhou
authors.initials: Z
authors.lastname: Mengge
authors.affiliation: Tianjin University of Traditional Chinese Medicine, Tianjin, 300071, People's Republic of China.
authors.forename: Chang
authors.initials: C
authors.lastname: Nianwei
authors.affiliation: Tianjin University of Traditional Chinese Medicine, Tianjin, 300071, People's Republic of China.
authors.forename: Pan
authors.initials: P
authors.lastname: Ye
authors.affiliation: State Key Laboratory of Medicinal Chemical Biology and College of Pharmacy, Nankai University, Tianjin, 300071, People's Republic of China.
authors.forename: Jiang
authors.initials: J
authors.lastname: Min
authors.affiliation: Second Affiliated Hospital of Tianjin University of Traditional Chinese Medicine, Tianjin, 300071, People's Republic of China.
authors.forename: Sun
authors.initials: S
authors.lastname: Zengtao
authors.affiliation: State Key Laboratory of Medicinal Chemical Biology and College of Pharmacy, Nankai University, Tianjin, 300071, People's Republic of China.
authors.forename: Bai
authors.initials: B
authors.lastname: Gang
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D057809:HEK293 Cells; D006801:Humans; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D016328:NF-kappa B / Q000037:antagonists & inhibitors*
chemical_list: D004365:Drugs, Chinese Herbal; D016328:NF-kappa B
keywords: Bufei Granule; NF-κB inhibitors; UPLC/QTOF-MS; constituent identification