Premium
Determination of tubuloside B by LC‐MS/MS and its application to a pharmacokinetic study in rats
Author(s) -
Yang Shenbao,
Qu Ruiying,
Sun Peilu,
Xiong Shan,
Yan Siyi,
Deng Zhipeng
Publication year - 2018
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.4138
Subject(s) - chemistry , chromatography , protein precipitation , ammonium acetate , selected reaction monitoring , mass spectrometry , pharmacokinetics , calibration curve , extraction (chemistry) , detection limit , liquid chromatography–mass spectrometry , tandem mass spectrometry , high performance liquid chromatography , medicine
Tubuloside B, a novel neuroprotective phenylethanoid, is a major active constituent of Cistanche tubulosa and Cistanche deserticola . A specific and sensitive liquid chromatography tandem mass spectrometry (LC‐MS/MS) method has been developed and validated for the quantification of tubuloside B in rat plasma. Sample preparation was conducted through a protein‐precipitation extraction with methanol using tubuloside A as internal standard (IS). Chromatographic separation was achieved using a Capcell Pak C 18 column (2.0 × 50 mm, 5 μm) with a mobile phase of methanol–10 m m ammonium acetate buffer (70:30, v/v) in an isocratic elution. Mass spectrometry analysis was performed in negative ionization mode with selected reaction monitoring transitions at m/z 665.1 → 160.9 for tubuloside B, and m/z 827.1 → 160.9 for IS. Calibration curves were linear over the range of 1.64–1640 ng/mL for plasma samples samples ( R 2 > 0.990). The lower limit of quantification (LLOQ) was 1.64 ng/mL. The intra‐ and inter‐day accuracy was between 92.3 and 113.0% with the RSD <9.23% at all LLOQ and quality control levels. Finally, this method was successfully applied in the pharmacokinetics study of tubuloside B after intravenous administration.