XIE Yan-xiang, JIANG Er-gang, DAI Tian-ming, et al. Simultaneous Determination of Four Main Effective Components in Extracts by LC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(18): 57-62.
XIE Yan-xiang, JIANG Er-gang, DAI Tian-ming, et al. Simultaneous Determination of Four Main Effective Components in Extracts by LC-MS/MS[J]. Chinese journal of experimental traditional medical formulae, 2018, 24(18): 57-62. DOI: 10.13422/j.cnki.syfjx.20181419.
Objective: To establish an LC-MS/MS method for simultaneous determination of the four effective components(paederosidic acid
paederoside
paederosidic acid methyl ester
and asperuloside) in Paederia scandens extracts. Method: A Venusil MP C18 column (2.10 mm×50 mm
5 μm)was used
with methanol(A)-water(B) as the mobile phase for gradient elution(0-0.3 min
10% A;0.3-0.8 min
10%-95%A;0.8-3.0 min
95%A;3.0-3.2 min
95%-10%A;3.2-4.5 min
10% A). The flow rate was 0.35 mL·min-1
the column temperature was room temperature
and the injection volume was 10 μL. Electrospray ionization(ESI) source was used. Quantization was performed using multiple reaction monitoring(MRM) mode and positive ionization condition. Mass spectrometric parameters of spectrometer and 4 effective components were optimized for testing and quantitative analysis. Result: Based on the instrument precision
linear range
repeatability
stability
recovery and other methodological validations
the results were in conformity with relevant standards of quantitative analysis. The calibration curves of paederosidic acid
paederosidic
methyl paederosidate and asperuloside showed a good linearity (r ≥ 0.994 7).The average recoveries of these four components were 90.8%-112.1%
with RSDs (n=6) of no more than 5.1%. Conclusion: The method is simple
rapid
accurate and reliable
and suitable for the quantitative analysis of four effective components in the extract of P. scandens.