A method was developed for the rapid and quantitative analysis of 30 veterinary drugs belonging to 17 classes (amphenicols (1), anthelmintics (1), cephalosporins (4), coccidiostats (1), lincosamides (1), macrolide (1), nitroimidazole (1), penicillins (3), phenylhydrazines (1), polypeptides (1), pyrethrins (1), quinolones (5), sulfonamides (3), tetracycline (3), neuroleptic agents (1), triazene trypanocidal agents (1), other. (1)) in feeds. The proposed method with a modified Quick Polar Pesticides (QuPPe) sample preparation was validated for the determination of 30 veterinary drugs in feed samples by liquid chromatography triple-quadrupole mass spectrometry (LC–MS/MS). The sample was extracted with methanol containing 1% acetic acid and purified by dispersive solid-phase extraction (d-SPE) with C18. Good linearity (r2 ≥ 0.98) was observed, and the LOQ values ranged from 10 to 200 µg/kg. Average recoveries ranged from 70.8 to 118.4%, and the relative standard deviation was ≤ 18.7%. This validated method was used in the determination of 30 veterinary drugs in 142 feed samples obtained from South Korea. The results show that lincomycin was present in only one of the tested feed samples, although it was detected at a value lower than the LOQ. In conclusion, this multi-residue method can be used for screening through the detection and quantitation of residual multiclass veterinary drugs in feed samples.
1 October 2024 in Journal of Agricultural and Food Chemistry
The plant-back intervals (PBIs) of imicyafos were investigated for rotational cultivation of lettuce and spinach in greenhouses. Imicyafos dissipation in soil and its plant uptake were evaluated by liquid chromatography-tandem mass spectrometry. Bioconcentration ratios (BCRs) were calculated by comparing the residues in plants to the initial residue in soil. The BCRs were used to calculate the soil acceptable residues (SARs) transferable to plants at the Positive List System (PLS) level. The number of days, PBIs for reaching SARs were obtained from the dissipation equation for imicyafos in soil. In soil, imicyafos followed first order dissipation kinetics (R2 = 0.975) with a half-life of 40.8 days. The BCRs ranged from 0.041 to 0.469 in the edible leaf parts of lettuce and 0.006 to 0.134 in those of spinach. The SARs ranged from 0.021 to 0.244 for lettuce and 0.075 to 1.667 mg kg−1 for spinach. The PBIs of imicyafos were estimated to be 213.9 to 357.3 days for lettuce and 100.8 to 283.6 days for spinach. This study suggests at least a minimum 1-year interval after the final application of imicyafos as a management method that complies with the PLS for the rotational cultivation of lettuce and spinach.