A rapid, accurate,
and selective analytical method to simultaneously
quantify 13 anticoagulant rodenticides in animal biological samples
was developed using high-performance liquid chromatography-tandem
mass spectrometry (HPLC-MS/MS) coupled with electrospray ionization
(ESI) in negative mode. Samples were extracted and purified based
on a modified QuEChERS (quick, easy, cheap, effective, rugged, safe)
sample preparation technique. The sample pH and the type of extraction
solvent and cleanup sorbent used to estimate the procedure’s
effectiveness were optimized. To improve the matrix effects and obtain
acceptable recoveries for 13 rodenticides, 0.1 mL/g biological sample
and 1 mL acetonitrile (or acetonitrile: EtOAc = 1:1/(v:v)) extraction
followed by Florisil/HC-C18/anhydrous Na
2
SO
4
(NaCl) cleanup under alkaline conditions was fully validated and
shown to be selective, precise, accurate, and linear in the range
from 1 to 100 ng/mL (g). The mean recoveries were between 52.78 and
110.69%, while the limits of detection and quantification ranged from
0.05 to 0.5 and 0.1–1 ng/mL (μg/kg), respectively. Ideal
soft matrix effects (≤20%) were observed for the vast majority
of rodenticides (>95%) showing either suppression or enhancement.
This method meets international criteria and is capable of simultaneously
identifying and quantifying anticoagulant rodenticides in animal blood
and tissues and can be suitable for the detection of poisoning cases
in the field of forensic or public health.