• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.124-134
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• 2019

An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

• Korean Journal of Soil Science and Fertilizer
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• v.7 no.2
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• pp.71-97
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• 1974

Many studies on the changes of the materials in the water-logged paddy soil have been reported, but there will be several problems to apply them on the field soil. The main differences between the method of soil packed in beaker or column tube to that of natural field furrow slice are with or without of the rice root and the effect of water percolation. On the other hand, the mechanism of the water percolation on the changes of material in the natural field furrow slice are gradually understood. The purpose of this experiment is to know the effect of the rice cultivation on the chemical and physical changes of material in the water-logged paddy soil. Obtained results are as follows. 1. The physical and chemical changes on the water-logged paddy soil in the non-planted control-plot were nearly the same as the beaker or column tube experiment, while in the planted plot, slightly altered patterns were observed. 2. The relation between the number of tillers and total cation, $Ca^{{+}{+}}$, $Mg^{{+}{+}}$, Fe and Mn in the leachate showed very high significance. T hisresult showed that the leaching of those cation was promoted by growing of the rice r- of the rice root. 3. On the other hand, the concentration of the potassium, silica and phosphorus in leachates was gradually decreased and that of $NH_4$-N could not detect after the stage of active tillering. These facts revealed that such components were absorbed by rice plant. 4. The highly significant correlation between the number of tillers and the concentration of the total cation, $Ca^{{+}{+}}$, $Mg^{{+}{+}}$, $Fe^{{+}{+}}$, Fe and Mn in the percolated water was observed except that of $Mg^{{+}{+}}$. It was also showed that the rice root promoted the leaching of those cation. 5. The very high significance in the correlation between $HCO_3{^-}$ and the number of tillers indicated that the higher activity of the rice root was, the more $HCO_3{^-}$ concentration in the leachate was increased. 6. The relationship between the $HCO_3{^-}$ and the total cation, $Ca^{{+}{+}}$, $Mg^{{+}{+}}$, $Fe^{{+}{+}}$, Fe and Mn was appeared very highly significant. $HCO_3{^-}$, the metabolite of the rice root, promoted the leaching of $Ca^{{+}{+}}$, $Mg^{{+}{+}}$, $Fe^{{+}{+}}$ and Mn. This fact might be a result that these cations were leached as the form of bicarbonate. 7. The iron in the leachate was the form of $Fe^{{+}{+}}$ and the correlation between $Fe^{{+}{+}}$ and $HCO_3{^-}$ was very highly significant. This result indicated that it seemed to be ferrous bicarbonate when it is leached out. 8. In the rhizosphere, ferrous iron was decreased gradually and the concentration of glucose was as high as 2 to 3 times in comparison with the other parts of the soil. These facts were the same as the previous reports in which rhizosphere was oxidized by the oxigen excreted from the root, and was enriched by the organic matter which was also excreted from the root and accumulated residues of the root. 9. ${\beta}$-Glucosidase and phosphatase activity in the rhizosphere was higher than that of the other parts of the soil. This facts might be attributed to the vigorous activity of microorganism in the rhizosphere where glucose concentration was high. 10. The pH in the leachate of the planted plot was lower than that of control, and the Eh on the planted soil was elevated in the last stage.