Development and Validation of Quantitative Ultraperformance Liquid Chromatography-Tandem Mass Spectrometry Assay for Anticoagulant Rodenticides in Liver

作者：Smith Lori L^*; Liang Boying; Booth Marcia C; Filigenzi Michael S; Tkachenko Andriy; Gaskill Cynthia L

来源：Journal of Agricultural and Food Chemistry, 2017, 65(31): 6682-6691.

DOI：10.1021/acs.jafc.7b02280

• rodenticides
• electrospray
• UPLC-MS/MS
• poisoning
• hydroxycoumarins
• indanediones
• dispersive SPE

Anticoagulant rodenticides (ARs) are used to control rodent populations; however, exposure to nontarget animals occurs. A sensitive and rugged quantitative method was developed, optimized, and validated for eight ARs in liver. Target analytes comprised two chemical classes: hydroxycoumarins (warfarin, coumachlor, dicoumarol, bromadiolone, brodifacoum, and difethialone) and indanediones (diphacinone and chlorophacinone). In this method, liver extracts were cleaned using dispersive solid phase extraction (d-SPE) to remove matrix interferences and analyzed by reverse phase ultraperformance liquid chromatographytandem mass spectrometry (UPLCMS/MS). Electrospray ionization in negative ion mode combined with multiple reaction monitoring (MRM) using a triple quadrupole mass spectrometer provided simultaneous confirmation and quantitation. Detection limits spanned 0.75-25 ng/g, and lower quantitation limits were established as 50 ng/g. Interassay method accuracy ranged from 92 to 110% across the analytical range (50-2500 ng/g) using matrix-matched calibrants with good repeatability (relative standard deviations 2-16%). Successful method transfer to another laboratory utilizing an Orbitrap mass analyzer, providing high mass accuracy, was assessed by good method reproducibility during blinded study analyses (6-29%; Horwitz ratios (HORRAT) <= 1.5).

• 出版日期2017-8-9