Determination of metribuzin in plant material by liquid chromatography tandem mass spectrometry
2015
Vuković, Gorica (Institute of Public Health, Belgrade (Serbia)) | Špirović, Bojana (Faculty of Agriculture, Belgrade-Zemun (Serbia)) | Bursić, Vojislava (Faculty of Agriculture, Novi Sad (Serbia)) | Vlajković, Jelena (Institute of Public Health, Belgrade (Serbia)) | Jovanović-Radovanov, Katarina (Faculty of Agriculture, Belgrade-Zemun (Serbia)
The goal of our study was the development and validation of the method for the determination of metribuzin residues in alfalfa (Medicago sativa). The metribuzin was extracted from plant samples using an extraction procedure based on the QuEChERS methodology modified for pigmented vegetables with the clean-up being modified by graphitized carbon black (GCB) sorbent. LC-MS/MS method with positive electron spray ionization (ESI) was used for the determination of metribuzin residues. The separation of the compounds from the plant extracts was achieved using reverse phase Zorbax C18 column (50mm×4.6mm i.d.) with 1.8 μm particle size. The identification and confirmation of metribuzin were based on the retention time and two typical monitoring transitions (MRM). The optimized analytical conditions were evaluated in terms of recovery, reproducibility, limit of quantification (LOQ) and linearity. The matrix influence on linearity and recovery and its effects on ionization was evaluated. The calibration range was from 0.010 to 0.100 mg/kg. The recovery was investigated at three levels of 0.01, 0.05 and 0.10 mg/kg and ranged from 84.3 to 93.2% (RSDs 4.47-5.37%).
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