Preliminary Analysis of Alkaloids from Ya'an Dao-di Herbs Cyathulae Radix by UPLC-Triple-TOF-MS
The alcohol extraction,salinization,dichlormethane extraction and concentration methods were adopted to extract and separate the total alkaloid from Cyathulae Radix and determine the optimal extraction and separation process.To establish a rapid qualitative analysis method for alkaloids in Cyathulae Radix by ultra-performance liquid chromatography triple quadrupole time-of-flight mass spectrometry(UPLC-Triple-TOF-MS),the Waters XSelect CSH-C18 column(2.1 mm×150 mm,1.7 μm)was used,the mobile phase was 0.1%aqueous formic acid solution(A)-acetonitrile(B)with gradient elution,the flow rate was 0.3 mL/min,the UV detection wavelength was 254 nm,the column temperature was 50℃,and the injection quantity was 3 μL.Electrospray ion source positive ion mode was adopted,and the scanning range was m/z 100～1 500.The sample data were collected by full scanning mode,and the alkaloid composition of Cyathulae Radix was quickly identified according to the information obtained by high-resolution mass spectrometry combined with secondary mass spectrometry.Two kinds of alkaloids in Cyathulae Radix were detected through the mass-to-charge ratio of molecular ion peaks and fragment ions,the Scifinder and Reaxy databases,and the literatures.The method of qualitative analysis of the alkaloids established in this study provides experimental basis for improving the quality control level and further elucidating the pharmacodynamic substance basis of Ya'an Dao-di herbs Cyathulae Radix.
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