ABSTRACT
The qualitative analysis of flavonoids in Coreopsis tinctoria was carried out by a combination of 2 D-TLC and HPLC-IT-TOF-MS. The separation was conducted on 2 D-TLC and a Phenomenex Kinetex Evo C_(18) column(2.1 mm×100 mm, 2.6 μm) with methanol-0.05% aqueous formic acid by gradient elution. Electrospray ionization-(ESI) source was applied and operated in both positive and negative ionization modes. Eighteen flavonoids including three flavonoids, one flavonol, nine flavonones, one flavanonol and four chalcones, were putatively identified from the flavone-enriched fraction of C. tinctoria. 2 D-TLC could separate the flavonoids from C. tinctoria. HPLC-IT-TOF-MS was able to quickly and accurately analyze the flavonoids in C. tinctoria. The results would provide experimental information for the efficacy material basis clarification of C. tinctoria.
Subject(s)
Chalcones , Chromatography, High Pressure Liquid , Coreopsis , Chemistry , Flavonoids , Phytochemicals , Plant Extracts , Spectrometry, Mass, Electrospray IonizationABSTRACT
Objective: To analyze the chemical constituent cluster of decoction of Sanguisorba Radix systemically by HPLC-IT-TOF/MS. Methods: The samples were scanned by broad spectrum of DAD detector and ionized in negative and positive environment of electron spray ionization. Results: A total of 82 chemical constituents (include isomers) were identified based on exact molecular mass, fragment, ultraviolet spectrum as well as the combination of the database. The chemical constituent cluster was composed of 69 phenolics, 8 triterpenes, 3 flavonoids, an organic acid, and a monoterpene glycoside, of which citric acid, brevifolin carboxylic acid, methoxybenzoic acid methyl ester-5-O-sulfate, isorhamnetin-sulfate, and methylellagic acid-sulfate, et al were firstly found in Sanguisorba Radix. Conclusion: The systemical analysis of the chemical constituent cluster of decoction of Sanguisorba Radix was able to supply a clear material basis for the further study of efficacy and pharmaceutical metabolism of Sanguisorba Radix.
ABSTRACT
Objective To in depth analyze the chemical profile of Marsdenia tenacissima using HPLC-IT-TOF-MS. Methods The pulverized materials were exacted with methanol in an ultrasonication manner and then separated on a Waters Acquity UPLC HSS T3 column (100 mm × 2.1 mm, 1.8 μm, Milford, MA, USA) that was eluted in gradient with 0.1% formic acid-acetonitrile. The data was collected using automatically triggered tandem mass spectrometric mode in positive/negative ionization polarities. The mass fragmentation patterns of polyoxypregnane derivatives were proposed using some authentic compounds. Results Six chlorogenic acid derivatives and 15 polyoxypregnane derivatives were definitely assigned by referring to reference components, whereas the other signals, including 100 polyoxypregnane derivatives, four flavonoids, and two chlorogenic acid derivatives were tentatively annotated via matching the acquired information with those achieved information and the proposed mass fragmentation rules. Conclusion The research efficiently and accurately analyzed the chemical profile of M. tenacissima using HPLC-IT-TOF-MS, which will provide meaningful information for the quality evaluation and the therapeutic mechanism investigation of M. tenacissima as well as its preparation Xiao-Ai-Ping.
ABSTRACT
OBJECTIVE: To investigate the impurity profile of raloxifene thus to lay a foundation for the establishment of drug quality standard. METHODS: HPLC-IT-TOF-MS was adopted to analyze destroyed raloxifene and reference substances of impurities. According to the mass spectrometry fragmentation patterns of known impurities, the structures of unknown impurities were speculated. RESULTS: Destroyed raloxifene totally produced three impurities, one of which was unknown. Based on the regular mass spectrometry fragmentation patterns of raloxifene and known impurities, the unknown impurity was speculated to be a sulfone that was generated through further oxidation of raloxifene. CONCLUSION: The methods and results of this study could lay a foundation for the impurity control during production and in vivo analysis of raloxifene.