Determination of 3-methoxysalicylamine levels in mouse plasma and tissue by liquid chromatography-tandem mass spectrometry: application to in vivo pharmacokinetics studies.

Zagol-Ikapitte I, Amarnath V, Jadhav S, Oates JA, Boutaud O
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 879 (15-16): 1098-104

PMID: 21489890 · PMCID: PMC3091354 · DOI:10.1016/j.jchromb.2011.03.026

We report the development of a sensitive liquid chromatography-tandem mass spectrometric assay to quantitate 3-methoxysalicylamine (3-MoSA) in biological samples. Derivatization with 1,1'-thiocarbonyldiimidazole followed by C(18) reverse-phase chromatography allowed the detection of both analyte and internal standard (hexylsalicylamine) using electrospray ionization and selected reaction monitoring (SRM) in positive ion mode. We monitored the transitions from m/z 196.7 to 65.1 and from m/z 250.1 to 77.1 for 3-MoSA and HxSA, respectively. The method is validated with respect to linearity (r(2)=0.995), precision (<17% RSD), recovery (100% for 3-MoSA and HxSA), and stability (77% after storage up to 7 month at -80°C). The LOD and LOQ were 16.12 and 48.87 μg/l, respectively and the LLOQ of 1 pg/ml. In addition, we used this assay to analyze the pharmacokinetics of 3-MoSA in mouse plasma and tissues following both intraperitoneal and oral administration, providing new information regarding the distribution of this compound in vivo.

Copyright © 2011 Elsevier B.V. All rights reserved.

MeSH Terms (14)

Administration, Oral Aminosalicylic Acids Animals Benzylamines Brain Brain Chemistry Chromatography, Liquid Injections, Intraperitoneal Linear Models Male Mice Mice, Inbred C57BL Tandem Mass Spectrometry Tissue Distribution

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