HPLC–MSn Analysis of Organic Acids and Glycosides in Qi-gui-yin Granules
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In this study, a systematic method was established for the global quality control of Qi-gui-yin granules, a five-herb Traditional Chinese Patent Medicine for the treatment of multiple drug-resistant Pseudomonas aeruginosa infections. Identification of organic acids and glycosides was conducted in this paper, and a fast and sensitive method based on high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was established for rapid separation and sensitive identification. Samples were separated on a Agilent SB C18 column (150 × 4.6 mm, 5 μm) by gradient elution using acetonitrile (A) and water–formic acid (B; 0.03 %, v/v) as mobile phase at a flow rate of 1.0 ml/min. Based on the mass spectra and retention time, 12 organic acids, 12 glycosides, and the other 7 compounds were identified or tentatively characterized. In this paper, five isomers of chlorogenic acid (caffeoylquinic acid) and four isomers of dicaffeoylquinic acid were reported; the fragment ions in mass spectrum of two isomers of chlorogenic acid were different from reported CQA, so we presume that they are new isomers of chlorogenic acid. Furthermore, it was found that the characteristic fragmentation reaction of glycosides was through the homolytic cleavage of the O-glycosidic bond to produce radical aglycone ion, and different glycoside compounds were suitable for different ionization conditions. Their fragmentation pathway was summarized, and the fragmentation pathway of all kinds of compounds was summarized to enrich the data. These characteristics can be used for structure elucidation of similar compounds.
KeywordsQi-gui-yin granules HPLC-MSn Chlorogenic acid Isomer
This study was supported by the National Natural Science Foundation of China (no. 81102777).
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