Abstract
A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction was validated for the extraction of seven coumarin anticoagulant rodenticides (ARs) and 36 pharmaceutical active compounds (PhACs) residues in soil samples using liquid chromatography tandem mass spectrometry (LC-MS/MS). The aim of this work was to develop a method for the monitoring of these compounds in agricultural lands as well as in forensic applications for the determination of ARs poisoning. As far as is known, this is the first time that a QuEChERS-based method is used for the extraction of ARs in soil, as well as on such a quantity of PhACs. A matrix effect study was carried out on samples of soil devoted to agriculture in the midland area of the Canary Islands (clay loam type). It was in house validated (accuracy, precision, and linearity) at seven spiked levels between 0.5 and 50 ng g−1. The limits of quantification (LOQ) ranged between 0.5 and 50.0 ng g−1 and the limits of detection (LOD) ranged from 0.024 to 6.25 ng g−1. The method was then successfully used for both the determination of the target analytes in the soils from the agricultural plots that had been irrigated with regenerated water, and in the soil collected from underneath wild bird carcasses (which had been the subject of forensic investigation).
Highlights
Soil is a very vulnerable pollution receptor environment from where pollutants can be emitted to other environmental compartments such as the atmosphere, ground or surface water, and biota [1]
The remaining analytes and procedural internal standards (P-IS) were analyzed in positive mode using precursor ions corresponding to [M + H]+ except for cefuroxime axetil, cloxacillin, eprinomectin, josamycin and penicillin V
Together with the protonated and deprotonated molecules already mentioned, the ionization process can produce a variety of adduct ions depending on the composition and concentration of mobile-phase additives and analytes, the pH, the mobile-phase flow rate, the temperature or even solvent impurities and glassware [63,64,65]
Summary
Soil is a very vulnerable pollution receptor environment from where pollutants can be emitted to other environmental compartments such as the atmosphere, ground or surface water, and biota [1]. Agricultural soil contamination can be direct and intended, thorough the application of pesticides to crops, or indirect and nonintended, mainly due to irrigation using regenerated waters and the use of compost of wastewater treatment plants (WWTPs) sludge. Both water and sewage sludge may contain various contaminants of emerging concern (CECs), including anticoagulant rodenticides (ARs) and pharmaceutical active compounds (PhACs). Some anticoagulants, such as warfarin or its analogues, are used in the medical treatment of blood hypercoagulability disorders [6] Taking this into account, ARs can reach wastewater through runoff after agricultural and livestock farming applications, bait solubilization in urban infrastructures or through urinary excretion from medical treatments [7,8]
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