BACKGROUND: Dithiocarbamte fungicides have been used in crop cultivation for diseases protection and treatment. And cultivated agricultrual products were used as feedstuff, and residual pesticides are likely to be absorbed and transferred to livestock. But the maximum residue limits (MRLs) were not established for dithiocarbate fungicides in livestock products, and thus an analysis method was developed and validated for dithiocarbamate fungicides to establish MRLs. METHODS AND RESULTS: Samples were prepared using CS 2 trap method and detected with UV/VIS spectrophotometer. Calibration line (0.1 ∼ 10 ㎍/mL) was linear with r 2 ⟩ 0.99. For validation, the recovery tests were carried out at three fortification levels (MLOQ, 10 MLOQ and 50 MLOQ) from livestock samples (egg, milk, beef, pork, and chicken). The results for mancozeb, propineb, and thiram ranged between 76.8 to 109.6%, 79.4 to 108.8%, and 80.2 to 107.8%, respectively and % RSD (relative standard deviation) values were below 9.5%. Furthermore, inter-laboratory analysis was performed to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-199340- , 200340- ) and MFDS guidelines (2016. This might be used as an official analytical method for determination of dithiocarbamate fungicides at established MRLs and monitoring.
This study was carried out to investigate the residual characteristics of flubendiamide in kale to establish pre-harvest residue limits (PHRL) and the removal efficiency according to the washing solvent and method. Field tests were conducted at two different greenhouses, field 1 (Anseong-si, Gyeonggi-do) and field 2 (Incheon-si, Gyeonggi-do). According to the safe use guidelines kale was sprayed with flubendiamide twice every 10 days and harvested 0 (after 2 h), 1, 2, 3, 5, 7 and 10 days after the final application. The biological half-live of flubendiamide in kale was calculated based on dissipation curves of the pesticide in samples analyzed by liquid chromatography coupled with tandem mass spectrometry. In the analysis, method limits of quantitation (MLOQ) were 0.01 mg/kg, and recoveries performed with two different fortification levels of 10 MLOQ and maximum residue limit (0.7 mg/kg) were 104.2±3.6 and 101.9±10.2%, respectively. The dissipation rate constant of flubendiamide in kales were 0.2437 at field 1 and 0.1981 at field 2. PHRL calculation equations obtained using the dissipation constants estimated as follows: if the residual concentration of flubendiamide in kale on 10 days before harvest is less than 8.0 mg/kg, the residual concentration on the harvest would be under MRL. The removal of flubendiamide from kale was the greatest when it was washed with vinegar (39.8%), followed by baking soda (31.7%), calcium powder (30.2%), neutral detergent (27.2%), and tap water (15.9%). The results of this study would be useful for both farmers and consumers to produce or consume safe agricultural products.
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