Characterization And Quantification Of Prim-O-Glucosylcimifugin In The Roots Of Saposhnikovia Divaricata And Its Medicinal Preparations By Liquid Chromatography-Ion Trap Mass Spectrometry

JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES(2013)

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摘要
A rapid and sensitive method for the identification and quantification of prim-O-glucosylcimifugin (POG) in Saposhnikovia divaricata is described. The POG standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MSn spectra. The electrospray ionization (ESI) mass spectral fragmentation pathway of POG was proposed and the ESI-MSn fragmentation behavior of POG was deduced in detail. The major product ion at m/z 307 belongs to dihydrofurochromone, which was formed by loss the glucose (162Da), and the characteristic eliminations of 18, 48, and 72 were observed. The loss of 18Da could arise from two different fragmentation pathways, and the observed ion was composed of a mixture of two different structural ions. Quantification of POG was assigned in positive-ion mode at a product ion at m/z 469307 by LC-MS. The LC-MS method was validated for linearity, sensitivity, accuracy, and precision, and then used to determine the content of the POG. Lastly, the LC-MS method was successfully applied to determine POG in real sample Saposhnikovia divaricata and its seven medicinal preparations in the first time.
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关键词
fragmentation pathways, liquid chromatographyion trap mass spectrometry, prim-O-glucosylcimifugin, Saposhnikovia divaricate
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