Multi-residue analysis of eight anticoagulant rodenticides in animal plasma and liver using liquid chromatography combined with heated electrospray ionization tandem mass spectrometry

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.…”

“…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].…”

Determination of seven anticoagulant rodenticides in human serum by ultra-performance liquid chromatography-mass spectrometry

“…Liquid chromatography-mass spectrometry (LC-MS) has high sensitivity and was used for analysis of bromadiolone in fox faeces, 10 chlorophacinone and diphacinone, 11 warfarin enantiomers in human plasma, 12,13 as well as bromadiolone, ocoumafen and brodifacoum in whole blood. 23 The detection limit of the targets for these methods was in the range of 0.07-3.21 mg L À1 . 23 The detection limit of the targets for these methods was in the range of 0.07-3.21 mg L À1 .…”

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

“…Residues are essentially absent from the poisoned animal's stomach content. Of the other internal tissues, the liver usually contains a high amount of these substances; thus, it can 12,15 Methodologies using HPLC with mass spectrometry detection 4,10,11,16 offer better sensitivity and versatility but require a more expensive experimental setup. None of the cited analytical methods presents complete validation studies for all of the anticoagulants that normally cause animal poisoning in southern Italy, including the region of Puglia e Basilicata.…”