Simultaneous measurement of indandione-type rodenticides in human serum by liquid chromatography-electrospray ionization-tandem mass spectrometry

Abstract

Measurement of indandione rodenticides is important in the diagnosis and treatment of accidental rodenticide ingestion. Current assays lack effective measurements for simultaneous analysis of the indandiones, especially the isomers. The intent of this study was to establish a novel and selective method for the simultaneous determination of indandione-type rodenticides (diphacinone, chlorophacinone, valone, and pindone) in human serum by liquid chromatography-electrospray ionization-tandem mass spectrometry. After addition of internal standard, the sample was extracted with 10% methanol in acetonitrile and cleaned by solid-phase extraction (SPE). The analytes were separated on a C18 rapid column and infused into an ion trap mass spectrometer in the negative electrospray ionization mode. The multiple-reaction monitoring ion pairs were m/z 339 →→ 167, m/z 373 →→ 201, m/z 229 →→ 145, m/z 229 →→ 172, and m/z 307 →→ 161 for diphacinone, chlorophacinone, valone, pindone, and IS, respectively. Recoveries were between 81.5 and 94.6%, and the limits of quantification were 0.2 to 0.5 ng/mL. Intra- and interday RSDs were less than 7.9 and 11.5%, respectively. The assay was linear in the range of 0.5-100.0 ng/mL with coefficients of determination (r2 > 0.99) for all analytes. The proposed method enables the unambiguous confirmation and quantification of the indandiones in both clinical and forensic specimens.