Simultaneous determination of six kinds of components in Gexia-Zhuyu Decoction by UPLC-MS/MS / 国际中医中药杂志

ABSTRACT

Objective:To develop an UPLC-MS/MS method for the determination of paeoniflorin, tetramethylpyrazine, nobiletin, paeonol, amygdalin and ligustilide in Gexia-Zhuyu Decoction. Methods:Isocratic elution was carried out with mobile phase consisting of methanol- 4 mM ammonium formate. The separation was performed on Waters XTerra MS C18 (2.1 mm × 50 mm, 3.5 μm), and the mass spectrometer was operated in the positive and negative ionization electrospray (ESI) mode using multiple monitoring (MRM) for analysis of six components. Quantitative analysis by external standard method. The precursor to product ion transitions monitored for paeoniflorin, tetramethylpyrazine, nobiletin, paeonol, amygdalin and ligustilide were m/z 525.0→449.1, 137.1→55.1, 403.0→373.0, 167.2→149.4, 456.5→323.3 and 191.1→91.1, respectively. Results:Paeoniflorin, tetramethylpyrazine, nobiletin, paeonol, amygdalin and ligustilide were all analyzed exactly, the linear ranges were 0.000 2-0.012 8, 0.000 8-0.051 2, 0.000 1-0.006 4, 0.000 2-0.012 8, 0.000 6-0.038 4, 0.000 1- 0.006 4 ng, respectively. The r were 0.999 3, 0.997 5, 0.999 6, 0.992 6, 0.995 5 and 0.999 1, respectively. The recoveries of six analytes ranged from 98.00% to 105.3% and the relative standard deviations ( RSD) were all below 2.47%. Conclusions:This method was sensitive, which could be applied for the determination of paeoniflorin, tetramethylpyrazine, nobiletin, paeonol, amygdalin and ligustilide in Gexia-Zhuyu Decoction.