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Development and validation of an LC/MS/MS method for simultaneous determination of shionone and epi ‐friedelinol in rat plasma for pharmacokinetic study after oral administration of Aster tataricus extract
Author(s) -
Yin DeFeng,
Zhou Kai,
Liu JiTao,
Hu Li,
Liu Ying,
Deng Jun,
Wang SongPing,
Xiong Ying,
Zhong Wu
Publication year - 2016
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.3658
Subject(s) - chromatography , chemistry , formic acid , electrospray ionization , selected reaction monitoring , extraction (chemistry) , mass spectrometry , calibration curve , pharmacokinetics , detection limit , analytical chemistry (journal) , tandem mass spectrometry , medicine
A rapid and sensitive liquid chromatography tandem mass spectrometry (LC/MS/MS) method was developed and validated using spinasterol as the internal standard (IS) for the simultaneous determination of shionone and epi ‐friedelinol in rat plasma. Plasma samples were pretreated using liquid–liquid extraction with ethyl ether. Chromatographic separation was achieved on a C 18 column (100 × 2.1 mm, 5 μm) with an isocratic elution consisting of acetonitrile–0.1% formic acid water (75:25, v / v ) at a flow rate of 0.30 mL/min. Detection was performed under the selected reaction monitoring scan using an electrospray ionization in the positive ion mode. The mass transitions were as follows: m / z 427.4 → 95.1 for shionone, m / z 411.4 → 205.2 for epi ‐friedelinol and m / z 395.3 → 105.2 for IS. All calibration curves exhibited good linearity ( r > 0.995) over the concentration range for both components. The intra‐ and inter‐day precisions at three QC and lower limit of quantitation levels were both <10.21% in terms of relative standard deviation, and the accuracy ranged from −7.13 to 8.02% in terms of relative error. The extraction recoveries of the compounds ranged from 82.07 to 89.81%. The developed method was successfully applied to the pharmacokinetic study of shionone and epi ‐friedelinol after oral administration of Aster tataricus extract to rats. Copyright © 2015 John Wiley & Sons, Ltd.