Development and validation of a highly sensitive LC-MS/MS-ESI method for the determination of nobiletin in rat plasma

application to a pharmacokinetic study

Avinash Kumar, V. C. Devaraj, Kalpesh C. Giri, Sanjeev Giri, Sriram Rajagopal, Ramesh Mullangi*

*Corresponding author for this work

Research output: Contribution to journalArticle

12 Citations (Scopus)

Abstract

A highly sensitive, rapid assay method has been developed and validated for the estimation of nobiletin in rat plasma with liquid chromatography coupled to tandem mass spectrometry with electrospray ionization in the positive-ion mode. The assay procedure involves extraction of nobiletin and citalopram (internal standard, IS) from rat plasma with liquid-liquid extraction. Chromatographic separation was achieved using an isocratic mobile phase (0.2% formic acid-acetonitrile, 20:80, v/v) at a flow rate of 0.6mL/min on an Atlantis dC18 column (maintained at 40±1°C) with a total run time of 2.0min. The MS/MS ion transitions monitored were 403.2→373.0 for nobiletin and 325.2→109.0 for IS. Method validation was performed as per Food and Drug Administration guidelines and the results met the acceptance criteria. The lower limit of quantitation achieved was 0.05ng/mL and the linearity range extended from 0.05 to 51.98ng/mL. The intra- and inter-day precisions were in the range of 1.96-14.3 and 6.21-12.1, respectively.

Original languageEnglish
Pages (from-to)1464-1471
Number of pages8
JournalBiomedical Chromatography
Volume26
Issue number12
DOIs
Publication statusPublished - Dec 2012
Externally publishedYes

Keywords

  • LC-MS/MS
  • method validation
  • nobiletin
  • pharmacokinetics
  • rat plasma

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