Comparative pharmacokinetic analysis of extracts of crude and wine-processed Dipsacus asper in rats by a sensitive ultra performance liquid chromatography-tandem mass spectrometry approach

摘要

The purpose of this study is to establish and validate an UPLC MS/MS approach to determine 4-caffeoylquinic acid, chlorogenic acid, 3,5-dicaffeoylquinic acid, loganic acid, loganin, sweroside, dipsacoside B and asperosaponin VI from extracts of crude and wine-processed Dipsacus asper in biological samples and apply the approach to a comparative pharmacokinetic study. A Waters BEH C-18 UPLC column was employed with acetonitrile/0.2% formic acid-water as mobile phases. The mass analysis was carried out in a triple quadrupole mass spectrometer using multiple reaction monitoring (MRM) with negative scan made. A one-step protein precipitation by acetonitrile was performed to extract the eight analytes from plasma. Our results revealed that all of the calibration curves displayed good linear regression (r(2) > 0.9990). The lower limits of quantification (LLOQ) were determined as 10.0, 9.6, 8.9, 9.1, 9.2, 9.8,10.1 and 9.8 ng/mL. The intra-day and inter-day precisions (RSD) of the eight compounds at high, medium and low levels were less than 4.94% and the bias of the accuracies ranged from -3.89% to 3.95%.The extraction recoveries of the eight compounds were from 90.4% to 100.2% and the matrix effects ranged from 89.3% to 100.1%. The stabilities of these compounds were investigated by analyzing six replicates of QC samples at three different concentrations following storage at 25 degrees C for 4 h, 80 degrees C for 30 days, three freeze -thaw cycles, and 4 degrees C for 24 h. All the samples showed satisfactory precision and accuracy after various stability tests. Pharmacokinetic parameters were estimated using a non-compartment model. Compared with the crude group, the parameters of C-max and AUC(0-t) of 4-caffeoylquinic acid, loganic acid, loganin and asperosaponin VI increased remarkably (p<0.05) after oral administration 'of the aqueous extract of wine-processed Dipsacus asper, indicating that wine-processing could enhance bioavailability of 4-caffeoylquinic acid, loganic acid, loganin and asperosaponin VI. (C) 2016 Elsevier B.V. All rights reserved.