Validation and application of multi-residue analysis of eight anticoagulant rodenticides by high-performance liquid chromatography with fluorimetric detection

Abstract

Abstract. Poisoning of domestic animals is frequently caused by anticoagulant rodenticides. Validation and applications of a rapid and reliable method for the simultaneous determination of 8 anticoagulant rodenticides (bromadiolone, brodifacoum, coumachlor, coumafuryl, coumatetralyl, difenacoum, flocoumafen, and warfarin) in baits and animal livers using highperformance liquid chromatography with fluorescence detection are reported herein. The methodology was validated by an in-house validation model at 2.5 mg/kg, which is the level commonly found in the tissues of poisoned domestic animals. The 8 anticoagulants can be determined at the concentration range of 1.25-100 mg/kg with determination coefficients higher than 0.992. A recovery value from 70% to 109% was observed for all the studied molecules. The results of the validation process demonstrate suitability for application in official analysis and for monitoring purposes of animal poisoning by anticoagulant rodenticides.

Simultaneous determination of nine anticoagulant rodenticides in soil and water by LC–ESI‐MS

“…CE and GC were employed in some cases, but these procedures were usually lengthy and more complicated, and for these reasons were not frequently employed. However, the most common separation technique used to determine the compounds is LC in reverse mode with UV or diode array detection (DAD) , fluorescence detection (FLD) or both , and more recently, LC coupled to MS . Furthermore, it should be mentioned that chiral stationary phases have also been employed to perform the LC analysis of CP and warfarin (W) , while in some cases monolithic stationary phases have been used to analyze W by liquid and affinity chromatography.…”

Analytical methods for determination of anticoagulant rodenticides in biological samples

“…Similar approaches, with combined LLE and SPE, have successfully been developed [11,12,14,25,26,31].…”

“…However these methods have low detection sensitivity mostly ranging from 10 to 100 ng/ mL. Similarly HPLC-FLD has also been employed for rodenticides detection [6][7][8][9][10][11][12][13][14]30]. Although fluorescence detection offers enhanced sensitivity for hydroxycoumarin based rodenticides, but it still requires an extensive sample clean-up.…”

“…Various organic solvents and their mixtures such as acetonitrileethylether [8], chloroform-acetone [10], acetone-diethyletherchloroform [11], acetonitrile-acetone [12], dichloromethaneacetone [14], 1-chlorobutane [18], ethyl acetate [19][20][21]28,32], acetone [22,23], acetonitrile [24][25][26]29] and methanol [30,33] were used to extract anticoagulant rodenticides from biological samples. Among all organic solvents used in LLE, acetonitrile-ethyl ether (9:1) [8] produced the highest recovery (92-109%) in plasma and liver tissues.…”

Metodología multiresiduo para análisis de rodenticidas en muestras ambientales

“…No cabe duda pues que la técnica habitualmente empleada es la cromatografía líquida en la que se siguen utilizando los detectores UVvisible (Ring, 2000, Vudathala, 2010 y fluorescencia (Armentano, 2012) o combinación de ambos; y en el caso de la espectrometría de masas existen distintas opciones, desde el cuadrupolo a las hibridaciones más actuales (Vandenbrouke, 2008;Zuo, 2010;Yan, 2012). En muy contadas ocasiones se emplean separaciones quirales previa a la detección por masas, lo más común ha sido estudiar los enantiómeros de la warfarina (Zuo, 2010), si bien dependiendo del selector quiral y el modo de operar se han propuesto también detectores UV (Locatelli, 2005) solos o acoplados en línea con detector de fluorescencia y dicroísmo circular (Takahshi, 1997), el empleo de la electroforesis capilar (Zhou, 2003), o la alternancia de columnas (Uno, 2007 (Shore ,2003).…”