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

J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Nov 15:1036-1037:33-41. doi: 10.1016/j.jchromb.2016.09.024. Epub 2016 Sep 30.

Abstract

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 C18 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 mode. 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 (r2>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 9.8ng/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°C for 4h, -80°C for 30days, three-freeze-thaw cycles, and 4°C for 24h. 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 Cmax and AUC0-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.

Keywords: Dipsacus asper; Pharmacokinetics; UPLC–MS/MS; Wine-processed.

Publication types

  • Comparative Study
  • Validation Study

MeSH terms

  • Animals
  • Chlorogenic Acid / analogs & derivatives
  • Chlorogenic Acid / analysis
  • Chlorogenic Acid / blood
  • Chlorogenic Acid / isolation & purification
  • Chromatography, High Pressure Liquid / methods*
  • Dipsacaceae / chemistry*
  • Drugs, Chinese Herbal / analysis
  • Drugs, Chinese Herbal / isolation & purification
  • Drugs, Chinese Herbal / pharmacokinetics
  • Iridoid Glucosides / analysis
  • Iridoid Glucosides / blood
  • Iridoid Glucosides / isolation & purification
  • Iridoids / analysis
  • Iridoids / blood
  • Iridoids / isolation & purification
  • Limit of Detection
  • Oleanolic Acid / analogs & derivatives
  • Oleanolic Acid / analysis
  • Oleanolic Acid / blood
  • Oleanolic Acid / isolation & purification
  • Plant Extracts / analysis
  • Plant Extracts / blood*
  • Plant Extracts / isolation & purification
  • Quinic Acid / analogs & derivatives
  • Quinic Acid / analysis
  • Quinic Acid / blood
  • Quinic Acid / isolation & purification
  • Rats
  • Rats, Sprague-Dawley
  • Saponins / analysis
  • Saponins / blood
  • Saponins / isolation & purification
  • Tandem Mass Spectrometry / methods*
  • Wine / analysis

Substances

  • Drugs, Chinese Herbal
  • Iridoid Glucosides
  • Iridoids
  • Plant Extracts
  • Saponins
  • akebia saponin D
  • caffeoylquinic acid
  • Quinic Acid
  • loganic acid
  • Chlorogenic Acid
  • dipsacoside B
  • Oleanolic Acid
  • loganin
  • sweroside
  • 3,5-dicaffeoylquinic acid