• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

• Applied Biological Chemistry
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• v.16 no.2
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• pp.99-111
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• 1973

Percentage recovery or fertilizer nitrogen, phosphorus and potassium by rice plant(Oriza sativa L.) were investigated at 8, 10, 12, 14 kg/10a of N, 6 kg of $P_2O_5$ and 8 kg of $K_2O$ application level in 1967 (51 places) and 1968 (32 places). Two types of nutrient contribution for the yield, that is, P type in which phosphorus firstly increases silicate uptake and secondly silicate increases nitrogen uptake, and K type in which potassium firstly increases P uptake and secondly P increases nitrogen uptake were postulated according to the following results from the correlation analyses (linear) between percentage recovery of fertilizer nutrient and grain or dry matter yields and nutrient uptake. 1. Percentage frequency of minus or zero recovery occurrence was 4% in nitrogen, 48% in phosphorus and 38% in potassium. The frequency distribution of percentage recovery appeared as a normal distribution curve with maximum at 30 to 40 recovery class in nitrogen, but appeared as a show distribution with maximum at below zero class in phosphorus and potassium. 2. Percentage recovery (including only above zero) was 33 in N (above 10kg/10a), 27 in P, 40 in K in 1967 and 40 in N, 20 in P, 46 in Kin 1968. Mean percentage recovery of two years including zero for zero or below zero was 33 in N, 13 in P and 27 in K. 3. Standard deviation of percentage recovery was greater than percentage recovery in P and K and annual variation of CV (coefficient of variation) was greatest in P. 4. The frequency of significant correlation between percentage recovery and grain or dry matter yield was highest in N and lowest in P. Percentage recovery of nitrogen at 10 kg level has significant correlation only with percentage recovery of P in 1967 and only with that of potassium in 1968. 5. The correlation between percentage recovery and dry matter yield of all treatments showed only significant in P in 1967, and only significant in K in 1968, Negative correlation coefficients between percentage recovery and grain or dry matter yield of no or minus fertilizer plots were shown only in K in 1967 and only in P in 1968 indicating that phosphorus fertilizer gave a distinct positive role in 1967 but somewhat' negative role in 1968 while potassium fertilizer worked positively in 1968 but somewhat negatively in 1967. 6. The correlation between percentage recovery of nutrient and grain yield showed similar tendency as with dry matter yield but lower coefficients. Thus the role of nutrients was more precisely expressed through dry matter yield. 7. Percentage recovery of N very frequently had significant correlation with nitrogen uptake of nitrogen applied plot, and significant negative correlation with nitrogen uptake of minus nitrogen plot, and less frequently had significant correlation with P, K and Si uptake of nitrogen applied plot. 8. Percentage recovery of P had significant correlation with Si uptake of all treatments and with N uptake of all treatments except minus phosphorus plot in 1967 indicating that phosphorus application firstly increases Si uptake and secondly silicate increases nitrogen uptake. Percentage recovery of P also frequently had significant correlation with P or K uptake of nitrogen applied plot. 9. Percentage recovery of K had significant correlation with P uptake of all treatments, N uptake of all treatments except minus phosphorus plot, and significant negative correlation with K uptake of minus K plot and with Si uptake of no fertilizer plot or the highest N applied plot in 1968, and negative correlation coefficient with P uptake of no fertilizer or minus nutrient plot in 1967. Percentage recovery of K had higher correlation coefficients with dry matter yield or grain yield than with K uptake. The above facts suggest that K application firstly increases P uptake and secondly phosphorus increases nitrogen uptake for dry matter yied. 10. Percentage recovery of N had significant higher correlation coefficient with grain yield or dry matter yield of minus K plot than with those of minus phosphorus plot, and had higher with those of fertilizer plot than with those of minus K plot. Similar tendency was observed between N uptake and percentage recovery of N among the above treatments. Percentage recovery of K had negative correlation coefficient with grain or-dry matter yield of no fertilizer plot or minus nutrient plot. These facts reveal that phosphorus increases nitrogen uptake and when phosphorus or nitrogen is insufficient potassium competatively inhibits nitrogen uptake. 11. Percentage recovery of N, Pand K had significant negative correlation with relative dry matter yield of minus phosphorus plot (yield of minus plot x 100/yield of complete plot; in 1967 and with relative grain yield of minus K plot in 1968. These results suggest that phosphorus affects tillering or vegetative phase more while potassium affects grain formation or Reproductive phase more, and that clearly show the annual difference of P and K fertilizer effect according to the weather. 12. The correlation between percentage recovery of fertilizer and the relative yield of minus nutrient plat or that of no fertilizer plot to that of minus nutrient plot indicated that nitrogen is the most effective factor for the production even in the minus P or K plot. 13. From the above facts it could be concluded that about 40 to 50 percen of paddy fields do rot require P or K fertilizer and even in the case of need the application amount should be greatly different according to field and weather of the year, especially in phosphorus.