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Determination of newly synthesized lipoic acid–niacin dimer in rat plasma by UPLC/electrospray ionization tandem mass spectrometry: assay development, validation and application to a pharmacokinetic study
Author(s) -
Chen Xiao,
Gao Jingwen,
Jiang Yiming,
Huang Ping,
Xie Yuhui,
Pi Rongbiao,
Zhu Shuzhen,
Yao Meicun
Publication year - 2014
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.3006
Subject(s) - chemistry , chromatography , electrospray ionization , tandem mass spectrometry , lipoic acid , mass spectrometry , selected reaction monitoring , pharmacokinetics , antioxidant , biochemistry , pharmacology , medicine
A simple, sensitive and specific ultra‐performance liquid chromatography/tandem mass spectrometry (UPLC‐MS/MS) method was developed to determine the newly synthesized compound lipoic acid–niacin dimer (N2L) in plasma. Plasma samples were precipitated by methanol using tetrahydropalmatine as internal standard. Chromatographic separation was achieved on an Acquity BEH C 18 (2.1 × 50 mm i.d., 1.7 µm) column; the mobile phase contains methanol and buffer solution (water with 0.5% formic acid and 10 mmol/L ammonium acetate). Multiple reaction monitoring ( m / z 353.9 → 148.6 for N2L and m / z 356.0 → 192.0 for internal standard) was performed for detection and quantification. The method was validated to be rapid, specific, accurate and precise over the concentration range of 1–750 ng/mL; N2L was not stable on the bench‐top or during freeze–freeze‐thaw cycles in plasma, but was stable in the stock solution and after preparation in the autosampler for 24 h. The utility of the assay was confirmed by pharmacokinetic study of N2L in rats. Copyright © 2013 John Wiley & Sons, Ltd.