RESUMEN
An analytical method was developed to determine the phenoxyacid herbicides 2,4-D, MCPA and mecoprop in kidney tissue from animals where poisoning is suspected. Samples were Soxhlet extracted using diethyl ether and the extracts cleaned-up using anion exchange solid phase extraction cartridges. Analysis was performed using liquid chromatography with negative-ion electrospray tandem mass spectrometry (LC-MS/MS). The method was evaluated by analysing control kidney samples fortified at 1 and 5 mg/kg. Mean recoveries ranged from 82 to 93% with relative standard deviations from 3.2 to 19%. The limit of detection was estimated to be 0.02 mg/kg.
Asunto(s)
Ácido 2,4-Diclorofenoxiacético/análisis , Ácido 2-Metil-4-clorofenoxiacético/análogos & derivados , Ácido 2-Metil-4-clorofenoxiacético/análisis , Cromatografía Liquida/métodos , Riñón/química , Extracción en Fase Sólida/métodos , Espectrometría de Masa por Ionización de Electrospray/métodos , Ácido 2,4-Diclorofenoxiacético/aislamiento & purificación , Ácido 2,4-Diclorofenoxiacético/envenenamiento , Ácido 2-Metil-4-clorofenoxiacético/aislamiento & purificación , Ácido 2-Metil-4-clorofenoxiacético/envenenamiento , Animales , Porcinos , Espectrometría de Masas en TándemRESUMEN
An analytical method employing clean up by high-performance gel permeation chromatography (HPGPC) and solid-phase extraction (SPE) on Florisil cartridges was developed to determine residues of eleven imidazole and triazole ergosterol-biosynthesis-inhibiting (EBI) fungicides in honeybee samples. Detection was by means of gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. The method was validated by fortifying control samples at levels of 0.01 and 0.05 micro g/bee. Mean recoveries for each analyte except imazalil were between 79 and 99% with relative standard deviations of 12.3% or less. Mean recoveries of imazalil were 51% at 0.01 micro g/bee and 81% at 0.05 micro g/bee. Limits of detection for the analytes investigated ranged from 0.005 to 0.001 micro g/bee.
Asunto(s)
Abejas/química , Fungicidas Industriales/análisis , Cromatografía de Gases y Espectrometría de Masas , Imidazoles/análisis , Residuos de Plaguicidas/análisis , Triazoles/análisis , Animales , Electrones , SolucionesRESUMEN
This study describes a generic biological screening assay designed to detect anticoagulant rodenticides based on their inhibitory action on the vitamin K epoxide reductase protein complex, resulting in an accumulation of under-carboxylated prothrombin or proteins induced by vitamin K antagonism (PIVKA-II). A combined cell culture/ELISA assay was optimized to measure PIVKA-II production by the human hepatoma HepG2 cell line cultured in the presence of anticoagulant rodenticides. The specificity and sensitivity of the assay was validated using 41 grain extracts containing representative concentrations of rodenticide or appropriate nonrodenticide control compounds. In all cases, PIVKA-II produced by HepG2 cells in response to grain extracts spiked with rodenticides was detected by ELISA, while PIVKA-II was not detected in supernatants collected from cells exposed to nonrodenticide controls. This represents a novel, class-specific biological assay for the detection of anticoagulant rodenticides present in contaminated grain.
Asunto(s)
Anticoagulantes/análisis , Bioensayo , Grano Comestible/química , Ensayo de Inmunoadsorción Enzimática/métodos , Indanos/farmacología , Rodenticidas/análisis , Anticoagulantes/farmacología , Biomarcadores/análisis , Carcinoma Hepatocelular , Línea Celular Tumoral , Cumarinas/análisis , Cumarinas/farmacología , Contaminación de Alimentos/análisis , Humanos , Indanos/análisis , Neoplasias Hepáticas , Organofosfatos/farmacología , Precursores de Proteínas/análisis , Precursores de Proteínas/biosíntesis , Protrombina/análisis , Protrombina/biosíntesis , Warfarina/análisis , Warfarina/farmacologíaRESUMEN
The United Kingdom Wildlife Incident Investigation Scheme (WIIS) investigates cases of suspected poisoning of wildlife, honey bees, and companion animals by pesticides. Together with field inquiries and veterinary post-mortem examinations, the analytical procedures presented here provide a comprehensive approach to the investigation of these cases. The paper covers selection of animal tissues for analysis and methods suitable for the analysis of honey bees and for various types of bait. Seven multiresidue methods cover around 130 pesticides, and methods are also described for a further 8 compounds. These methods are currently used on samples submitted to the Scheme in England and Wales.