Investigation of JinKui ShenQi Pills by Ultraviolet Spectra and Tandem Mass Spectrometry
LI Wen-lan1,2,SUN Zhi1,CHENG Bin1,JI Yu-bin1,BAI Jing1
1.Center of Research and Development on Life Sciences and Environmental Sciences, Harbin University of Commerce, Harbin 150076, China 2.Engineering Research Center of Natural Anticancer Drugs, Ministry of Education, Harbin 150076, China
Abstract：On the base of establishing the fingerprint of JinKui ShenQi pills, the ultraviolet spectra-mass spectrometry/mass spectrometry, method was used to identify the fingerprint.Seperation was performed on the Symmetry ShieldTM RP18 (5 μm, 4.6 mm×15 mm) analytical column with mobile phase consisting of 1% acetic acid and acetonitrile with gradient elute at the flow rate of 1.0 mL·min-1, and the ultraviolet detection wavelength was set at 248 nm.Using the above-mentioned chromatographic condition，the fingerprint of different samples was established and the same fingerprint was defined.The fingerprints of different samples were compared with similarity evaluation software published by Pharmacopeia committee codex (2004A).The mass spectrograph with API-ESI ionization source was used, setting the flow rate at 0.5 mL·min-1 after splitting stream.The pressure of atomization room was 50 Psi, the flow rate of dry gas was 9.0 L·min-1, the capillary voltage was 4 kV, and the transmission voltage was 70 V.The negative scanner mode was chosen, scan scope was 100-2 000, using ion trap to analyze quasi-molecular ion peak and the selected fragment ion, and TIC chromatography and second order mass chromatogram were recorded.The major constituents among in JinKui ShenQi pills from different origins were separated well by HPLC.Although there was difference among different origins, they showed nineteen identical characteristic absorption bands.Three fingerprints chemical compositions such as loganin, cinnamal and paeonol were identified based on the retention time and ultraviolet spectra of standard preparation.According to their ultraviolet spectra, molecularweight and fragmentation information, ten peaks in the fingerprint were identified by ultraviolet spectroscopy-mass, spectrometry/massg spectrometry.They are 1,2,3-tri-O-galloyl-glucose, loganin, paeoniflorin, 1,2,3,6-tetro-O-galloyl-glucose, soya-cerebroside, cornuside, and PGG, benzoyl-oxypaeoniflorin.The result showed that the presented fingerprint of JinKui ShenQi pills contained plenty of information quite valuable for the quality evaluation as well as chemical characterization of JinKui ShenQi pills.
Key words：JinKui ShenQi pills;UV spectroscopy and tandem mass spectrometric;Fingerprints
李文兰1,2,孙志1,程斌1,季宇彬1,白晶1. 金匮肾气丸的紫外光谱-质谱/质谱研究[J]. 光谱学与光谱分析, 2008, 28(08): 1914-1918.
LI Wen-lan1,2,SUN Zhi1,CHENG Bin1,JI Yu-bin1,BAI Jing1. Investigation of JinKui ShenQi Pills by Ultraviolet Spectra and Tandem Mass Spectrometry. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2008, 28(08): 1914-1918.
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