Determination of 3 Cephalotaxus Alkaloids and 2 Harringtonic Acids in Cephalotaxus hainanensis by UPLC-MS
The contents and distributions of anti-cancer drugs in Cephalotaxus hainanensis,including harringto-nine,homoharringtonine and their direct precursors of cephalotaxine,harringtonic acid and homoharringtonic acid were explored in this study.Ultrasonic bath and methanol were used to extract alkaloids and their precursors from Cephalotaxus hainanensis sample,and a UPLC-MS method was established for the detection.Chromatographic conditions:the chromatographic column Agilent Infinity Lab EC-C18(2.1 mm×100 mm,2.7 μm)was gradient eluted with a mobile phase of 0.1％v/v formic acid in water and acetonitrile,detection wavelength of 291 nm,column temperature of 30 ℃,injection volume of 2 μL,and flow rate of 0.3 mL/min.Mass spectrometric conditions:the mass spectrometer was operated in Full MS/AIF mode with a scan collision energy of 35 eV,spray voltage 3.5 kV,the temperature of that ion transmission tube 275 ℃,auxiliary gas heating temperature 350 ℃,sheath gas flow rate 35 arb,auxiliary gas flow rate 15 arb,sweep gas flow rate 5 arb;the auxiliary gas,sheath gas and sweep gas are high purity nitrogen(N2).Three alkaloids were detected in positive mode,and two harringtonine acids were de-tected in negative mode.The newly established UPLC-MS detection method can separate and detect various target compounds within 16 min characterized with simple operation,precision and reliability,which can provide a refer-ence for qualitative and quantitative analysis of harringtonine,homoharringtonine and their precursors in Cephalotaxus hainanensis.In addition,the contents of harringtonine、homoharringtonine and their corresponding precursor harringtonine acids in different tissues are positive correlated with growing years.
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