Analysis of anticoagulant rodenticide residues in Microtus arvalis tissues by liquid chromatography with diode array, fluorescence and mass spectrometry detection

Analytical methods for determination of anticoagulant rodenticides in biological samples

“…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.…”

“…HPLC-UV detection has been used for analysis of diphacinone, chlorophacinone in biological fluids and tissues [9][10][11]13,30], difethialone, pindone, coumafuryl and warfarin in blood, plasma and liver [13,15,16], and warfarin, coumatetralyl, crimidine and bromadiolone in blood and urine [17]. However these methods have low detection sensitivity mostly ranging from 10 to 100 ng/ mL.…”

“…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.…”

“…Anticoagulant rodenticides (coumatetralyl, difenacoum, brodifacoum, bromadiolone, warfarin, chlorophacinone, coumafuryl, diphacinone, coumachlor, difethialone, flocoumafen and dicoumarol) were quantitated from biological samples such as plasma, serum, blood, liver and hair by various techniques of LC-MS. Electrospray ionization (ESI) in negative mode was extensively used for ionization of analytes. In reported LC-MS and LC-MS/MS methods, elution was performed by isocratic [20,21,26,30] as well as by gradient manner [18,19,[22][23][24][25][27][28][29][31][32][33]. The MS parameters used in these methods were capillary voltage (2.5-3.0 kV), capillary exit voltage (À135 to À205 V), drying temperature (325-350 8C), high purity (99.999%) dry nitrogen gas ( [29] performed using helium as collision gas at a pressure of 1.22 Â 10 À5 mbar [18][19][20][21][22][23][24][25][26][27][28][29][30][31][32][33].…”

“…Acquisition methods including selected ion monitoring (SIM), multiple reaction monitoring (MRM) and selected reaction monitoring (SRM) have been applied to the LC-MS and LC-MS/MS analysis of anticoagulant rodenticides in biological samples (Table 4). Jin et al [21] determined the flocoumafen and brodifacoum from whole blood with relatively better recovery (78.0-83.7%) and sensitivity (LOQ: 0.05-0.1 ng/mL) when compared with other isocratic elution methods [20,26,30]. Among the reported methods of gradient elution, Dong et al [33] worked on determination of seven rodenticides in human serum by UPLC-MS and have demonstrated higher recovery (77.3-98.2%).…”