Analytical methods for determination of anticoagulant rodenticides in biological samples

Imran, Muhammad; Shafi, Humera; Wattoo, Sardar Ali; Chaudhary, Muhammad Taimoor; Usman, Hafiz Faisal

doi:10.1016/j.forsciint.2015.06.008

Cited by 29 publications

(18 citation statements)

References 41 publications

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“…Numerous Liquid Chromatography on line with two dimensional Mass Spectrometry (LC-MS/MS) multi-residue methods have been published to quantify ARs in biological or environmental matrices [18][19][20][21][22][23]. Imran et al [24] published a review of analytical methods for the determination of anticoagulant rodenticides in biological samples; none of them reported the quantification of SGARs diastereoisomers, even less SGARs enantiomers. Consequently no data is today available on SGARs diastereoisomers/enantiomers residues in rodent or non target wildlife after using them as biocide or plant protection purposes, although secondary poisoning evidences and large scale surveys have been documented in the past recent years [5][6][7][8][9][10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Core-shell LC–MS/MS method for quantification of second generation anticoagulant rodenticides diastereoisomers in rat liver in relationship with exposure of wild rats

Fourel

Damin-Pernik

Benoît

et al. 2017

Journal of Chromatography B

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Second generation anticoagulant rodenticides (SGARs), pesticides used worldwide to control rodent populations, exist in two diastereoisomer chemical species because they own two stereogenic centers. A core-shell LC-MS/MS multi-residue method for comprehensive quantitative analysis of the diastereoisomers of five SGARs as well as three first generation anticoagulant rodenticide molecules has been fully validated in liver of rats according to a bioanalytical guideline. A core-shell column (superficially porous particles) has been chosen for its ability to separate the diastereomers of bromadiolone, difenacoum, brodifacoum, flocoumafen and difethialone and for its robustness to rat liver extracts. The highly selective chromatographic separation of the diastereoisomers contributes to good signal to noise ratios and then enhances the sensitivity of the method compared to the ones of fully porous columns. An elution gradient has been optimized with 10mM ammonium acetate and acetonitrile as aqueous/organic mobile phase respectively. Triple quadrupole mass detector has been used to achieve specifity and LLOQ from 0.92 to 2.2ng/g for each diastereoisomer, or first generation anticoagulant rodenticides. Then we evidenced diastereoisomeric ratios in liver of rats issued from not controlled exposure of wild rats (Rattus norvegicus) trapped in a French Parisian park through a campaign of rodent eradication. We compared them to diastereoisomeric ratios in SGARs commercial baits that contain both isomers, and showed that one of the two diastereoiomers had nearly disappeared in liver of rats. The proportions of cis-bromadiolone and trans-difenacoum were really lowered compared to the baits: 5/7 and 9/12 rats had only trans-bromadiolone and cis-difenacoum hepatic residues respectively. Liver persistence of the two diastereoisomers of bromadiolone and difenacoum was different due to differences in their pharmacokinetics in wild rats. The new core-shell LC-MS/MS method is particularly well adapted for further exploration of diastereoisomers ratios in rodent and predatory wildlife biological samples in order to evaluate ecological consequences of actual baits, to explore new formulated baits with a good balance between efficacity (ability to kill rodents) and diastereoisomers persistence, and hopefully to mitigate exposure of non-target species.

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Section: Introductionmentioning

confidence: 99%

Core-shell LC–MS/MS method for quantification of second generation anticoagulant rodenticides diastereoisomers in rat liver in relationship with exposure of wild rats

Fourel

Damin-Pernik

Benoît

et al. 2017

Journal of Chromatography B

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“…Intentional or accidental poisonings with strychnine occur mainly in small animals, especially dogs and occasionally cats, and rarely in farm animals. From animals, for the purposes of toxicological examinations, the most frequently used matrices are stomach contents, blood, and liver, whereas from environmental samples they are baits and feeds [4,5,6,7,8,9,10,11,12]. Cases of strychnine poisoning are usually acute or hyperacute.…”

Section: Introductionmentioning

confidence: 99%

The Usefulness of MS3 to Confirm Poisoning on the Example of Dog Poisoning with Strychnine

2019

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Strychnine is an alkaloid with strong toxic properties. Poisoning results in muscular contractions and death through asphyxiation. Intentional or accidental poisonings with strychnine occur mainly in small animals, especially dogs and occasionally cats. Strychnine can be detected in the liver or stomach contents. Unfortunately, the determination of strychnine in these matrices, especially in postmortem examination, is subject to a significant matrix effect that makes it difficult to confirm the presence of the substance being determined. Therefore, we developed a new liquid chromatography method combined with mass spectrometry. One-gram homogenized samples were extracted and partitioned after adding acetonitrile and 5-mol solution of ammonium acetate. After extraction, the samples were analyzed using high-pressure liquid chromatography-MS/MS/MS. The results of validation fulfil the requirement of the confirmatory criteria according to SANTE/11945/2015 regarding apparent recoveries (98.97% to 104.0%), repeatability (2.9%–4.1%), and within-laboratory reproducibility (3.3%–4.6%). The method can be successfully applied to confirm strychnine poisoning cases.

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“…Furthermore, there are numerous AR substances that may enter the environment and so a comprehensive assessment of the presence of AR requires very sensitive and accurate multi-methods, covering a wide range of different ARs. Several analytical approaches for multi-methods for the quantitative determination of AR in biological samples have been developed, such as liquid chromatography (LC) and also ion chromatography (IC) coupled to tandem mass spectrometry (MS/MS) (Bidny et al 2015 , Chen et al 2009 , Jin et al 2009 , Jin et al 2008 , Marek and Koskinen 2007 ), two-dimensional LC coupled to MS/MS (Marsalek et al 2015 ), IC coupled to fluorescence detection (Jin et al 2007 ), methods using high resolution MS (Schaff and Montgomery 2013 ), and some other strategies that are presented in a review by Imran et al ( 2015 ). Available analytical methods are so far hampered by the number of captured AR, as well as high limits of detection caused by complex biological and environmental matrices that are in contrast to low relevant environmental concentrations.…”

Section: Introductionmentioning

confidence: 99%

First evidence of anticoagulant rodenticides in fish and suspended particulate matter: spatial and temporal distribution in German freshwater aquatic systems

Kotthoff

Rüdel

Jürling

et al. 2018

Environ Sci Pollut Res

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Anticoagulant rodenticides (ARs) have been used for decades for rodent control worldwide. Research on the exposure of the environment and accumulation of these active substances in biota has been focused on terrestrial food webs, but few data are available on the impact of ARs on aquatic systems and water organisms. To fill this gap, we analyzed liver samples of bream (Abramis brama) and co-located suspended particulate matter (SPM) from the German Environmental Specimen Bank (ESB). An appropriate method was developed for the determination of eight different ARs, including first-and second-generation ARs, in fish liver and SPM. Applying this method to bream liver samples from 17 and 18 sampling locations of the years 2011 and 2015, respectively, five ARs were found at levels above limits of quantifications (LOQs, 0.2 to 2 μg kg −1 ). For 2015, brodifacoum was detected in 88% of the samples with a maximum concentration of 12.5 μg kg −1 . Moreover, difenacoum, bromadiolone, difethialone, and flocoumafen were detected in some samples above LOQ. In contrast, no first generation AR was detected in the ESB samples. In SPM, only bromadiolone could be detected in 56% of the samples at levels up to 9.24 μg kg −1 . A temporal trend analysis of bream liver from two sampling locations over a period of up to 23 years revealed a significant trend for brodifacoum at one of the sampling locations.

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Analytical methods for determination of anticoagulant rodenticides in biological samples

Cited by 29 publications

References 41 publications

Core-shell LC–MS/MS method for quantification of second generation anticoagulant rodenticides diastereoisomers in rat liver in relationship with exposure of wild rats

Core-shell LC–MS/MS method for quantification of second generation anticoagulant rodenticides diastereoisomers in rat liver in relationship with exposure of wild rats

The Usefulness of MS3 to Confirm Poisoning on the Example of Dog Poisoning with Strychnine

First evidence of anticoagulant rodenticides in fish and suspended particulate matter: spatial and temporal distribution in German freshwater aquatic systems

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