Journal Article

Rapid Identification and Determination of the Rodenticide Valone in Serum by High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Mei-qiang Cai, Xiao-hong Chen, Xiao-kun OuYang and Mi-cong Jin

in Journal of Analytical Toxicology

Volume 33, issue 2, pages 104-108
Published in print March 2009 | ISSN: 0146-4760
Published online March 2009 | e-ISSN: 1945-2403 | DOI: http://dx.doi.org/10.1093/jat/33.2.104
Rapid Identification and Determination of the Rodenticide Valone in Serum by High-Performance Liquid Chromatography-Tandem Mass Spectrometry

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Valone is a chronic anticoagulant rodenticide that has come into wide use in China. Current literature lacks analytical methods for the determination of valone. In this paper, a sensitive and selective assay was established for the identification and quantification of valone in serum by liquid chromatography-tandem mass spectrometry. After addition of the internal standard, warfarin, serum samples were extracted with 10% methanol in acetonitrile and cleaned using Oasis HLB solid-phase extraction (SPE) cartridges. The compounds were separated on an Agilent SB C18 column with a mobile phase of methanol/acetic acid-ammonium acetate (5 mmol/L, pH 6.3) (75:25, v/v). Detection was performed by electrospray ionization ion trap mass spectrometry in the negative multiple reaction monitoring mode. The transition ions of m/z 229 → 145 and m/z 307 → 161 were selected for quantification of valone and the internal standard, respectively. The overall extraction efficiency was between 81.1% and 91.1%. The limit of quantification was 0.5 ng/mL. Regression analysis of the calibration data revealed good correlation (r2 > 0.99) for valone. Intra- and interday precisions for quality-control samples were less than 7.8% and 12.8%, respectively. This method combines a rapid SPE procedure with an extremely fast chromatographic analysis, which is especially advantageous or clinical laboratories.

Journal Article.  0 words. 

Subjects: Medical Toxicology ; Toxicology (Non-medical)

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