Simultaneous Determination of Eight Anticoagulant Rodenticides in Blood Serum and Liver

Abstract

A liquid chromatographic method was developed for the analysis of indandione and 4-hydroxycoumarin anticoagulant rodenticides in blood serum and liver. The method enabled the measurement of serum and liver concentrations of eight anticoagulant rodenticides: brodifacoum, bromadiolone, chlorophacinone, coumafuryl, coumatetralyl, diphacinone, difenacoum, and warfarin. Anticoagulants were extracted from serum and liver with acetonitrile. Extracts were applied to solid-phase extraction columns, which contained mixed packings. Column eluates were evaporated to dryness, reconstituted, and subjected to reversed-phase liquid chromatography. Hydroxycoumarins were detected by fluorescence at an excitation wavelength of 318 nm and an emission wavelength of 390 nm. Indandiones were detected by UV absorption at 285 nm. Extraction efficiencies of greater than 75% for serum and greater than 69% for liver were obtained. The within-run precision (CV) ranged from 2.4 to 8.6% for serum and 2.6 to 8.7% for liver. The between-run precision (CV) ranged from 1.5 to 12.2% for serum and from 2.1 to 11.8% for liver. Hydroxycoumarin rodenticides were detected at 1 ng/mL of serum and 1 ng/g of liver. Indandiones were detected at 10 ng/mL of serum and 10 ng/g of liver.

Luminescence methods in pesticide analysis. Applications to the environment

“…Therefore, the fluorescence properties of anticoagulant rodenticides including indanediones [19][20][21] and coumarins [19][20][21][22][23][24][25][26][27][28][29], carbamate insecticides such as aminocarb [30], bendiocarb [19,21,31], benomyl [31,32], carbaryl [31,[33][34][35][36] and carbofuran [35,36], and some organophosphorus insecticides, including coumaphos [31] and pirimiphos-methyl [19,21], and other classes of pesticides [31] have been investigated. For example, Krause [31] has selected 75 pesticides, metabolites and a number of industrial chemicals for HPLC studies, based on their known fluorescence or on chemical structures indicating possible fluorescence.…”

“…Herbicides [37][38][39], and fungicides [40][41][42][43] have been also analysed by direct fluorimetry. In most cases, the pesticide fluorimetric detection has been performed on solid substrates by thin layer chromatography (TLC) [32,44] or in combination with dynamic systems including HPLC [20,[22][23][24][25][26][27][28][29][30][31][33][34][35][36][37][40][41][42][45][46][47][48] and flow injection analysis (FIA) [21,43]. For instance Garcia and Aaron [43] applied FIA with spectrofluorimetric detection for determining fungicides such as thiabendazole and fuberidazole at the ng ml -1 level in river waters (Fig.…”

Superwarfarins

“…It is a yellowish powder and stable up to 200°C (Chalermchaikit et al, 1993). It is very soluble in dimethylformamide (730 g/L), but less soluble in ethyl acetate (25 g/L), and ethanol (8.2 g/L), and sparingly soluble in water (0.019 g/L).…”

Difficultés analytiques de la caractérisation des pesticides dans le sang

“…[25] en 1993 ont développé une méthode d'analyse de 8 rodenticides anticoagulants dérivés de la 4-hydroxycoumarine et de l'indanedione dans le sérum. Les anticoagulants sont extraits du sérum par l'acétonitrile.…”