Determination of bromadiolone in whole blood by high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry

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

“…Recently, several liquid chromatography coupled to electrospray ionization mass spectrometry methods (LC-ESI-MS) have been described for the determination of multiple coumarin and indandione anticoagulant rodenticides in diverse matrices. Jin and Chen [16] described the rapid determination of the three anticoagulant rodenticides bromadiolone, flocoumafen and brodifacoum in whole blood by LC-ESI-MS. HLPC-MS/MS assays were developed for the determination of flocoumafen and brodifacoum [17], coumatetralyl [18] and bromadiolone [19], at trace levels in whole blood which can be of use in the diagnosis of poisoned human beings. Marek and Koskinen [20] on the other hand described LC-ESI-MS/MS as a method to confirm and quantify seven anticoagulant rodenticides in diverse matrices such as animal feed stocks, baits and liquid matrices.…”

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.…”

“…Among all organic solvents used in LLE, acetonitrile-ethyl ether (9:1) [8] produced the highest recovery (92-109%) in plasma and liver tissues. However use of ethyl acetate [19][20][21]28] gave minimum recovery ranging from 54.3 to 96% (Tables 2 and 3). …”

“…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%).…”