• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.140-147
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• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• 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.

• Korean Journal of Food Science and Technology
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• v.53 no.2
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• pp.195-203
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• 2021

Aureobasidium pullulans, a black yeast, produces pullulan, a linear α-glucan composed of maltotriose repeating units linked by α(1→6)-glycosidic linkages. Pullulan can be widely used in food, cosmetic, and biotechnology industries. In this study, we isolated eight strains of A. pullulans from Forsythia koreana, Magnolia kobus DC., Spiraea prunifolia var. simpliciflora, Cornus officinalis, Cerasus, and Hippophae rhamnoides. Among them, A. pullulans MR was selected as the best pullulan producer. The effects of a carbon source, a nitrogen source, and pH on pullulan production were examined. The optimal cultivation conditions for pullulan production by A. pullulans MR were determined by response surface methodology as 15% sucrose, 0.4% soy peptone, and an initial pH of 7 at 26℃. Under these conditions, the predicted pullulan production was 47.6 g/L, which was very close to the experimental data (48.9 g/L).

• Korean Journal of Environmental Agriculture
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• v.41 no.2
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• pp.82-94
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• 2022

BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO₄, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C₁₈) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO₄. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

• Journal of the Korea Organic Resources Recycling Association
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• v.31 no.1
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• pp.35-45
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• 2023

In this study, the sludge formation in the wastewater drain from the advanced packaging process mechanisms are revealed as well as the key factors, materials, and sludge prevention methods using surfactant. Compared with that of conventional packaging process, advanced packaging process employ similar process to the semiconductor fabrication process, and thus many processes may generate wastewater. In specific, a large amount of wastewater may generate during the carrier wafer bonding, photo, development, and carrier wafer debonding processes. In order to identify the key factors for the formation of sludge during the advanced packaging process, six types of chemicals including bonding glue, HMDS, photoresist (PR), PR developer, debonding cleaner, and water are utilized and mixing evaluation is assessed. As a result, it is confirmed that the black solid sludge is formed, which is originated by the sludge seed formation by hydrolysis/dehydration reaction of HMDS and sludge growth via hydrophobic-hydrophobic binding with sludge seed and PR. For the sludge prevention investigation, three surfactants of CTAB, PEG, and shampoo are mixed with the key materials of sludge, and it is confirmed that the sludge formations are successfully suppressed. The underlying mechanism behind the sludge formation is that the carbon tails of the surfactant bind to PR with hydrophobic-hydrophobic interaction and inhibit the reaction with HMDS-based slurry seeds to prevent the sludge formation. In this regard, it is expected that various problems like clogging in drains and pipes during the advanced packaging process may effectively solve by the injection of surfactants into the drains.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.10 no.4
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• pp.181-195
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• 2005

To study the effects of aquaculture activity of marine cage fish farms on marine environment, field researches including hydrography, sediment, benthos and trap experiment at the marine cage fish farms(Site A) around estuaries of Tongyeong city were carried out during June $26\~27$, 2003. A simulation using numerical model-DEPOMOD was conducted to predict the solid deposition from fish cage and to assess the probable solid deposition, and the efficiency of environmental management of marine cage fish farms was studied. The marine cage fish farms cultured mainly common sea bass (Lateolabrax japonicus), red seabream (Pagrus major), striped breakperch (Oplegnathus fasciatus) and black rockfish(Sebastes schlegeli), and total amount of cultured fish of the Site A were 23.1MT. The amount of husbandry fish by unit area(and volume) of the fish cage was $43.0kg\;m^{-2}(6.1kg\;m^{-3})$. The daily mean amounts of food fed by unit biomass and cage area were $30.8g\;kg^{-1}day^{-1},\;1.32kg\;m^{-2}day^{-1},$ respectively, at the Site A. The concentration of ORP of the sediment below the center at the Site A was -334.6 mV and the concentrations of AVS, COD, Carbon and Nitrogen were $0.43mg\;g^{-1}dry,\;17.75mg\;g^{-1}dry,\;10.19mg\;g^{-1}dry\;and\;3.49mg\;g^{-1}dry$, respectively. Capitella capitata was dominant benthic species which occupied $57.8\%$ of total species, and the Infaunal Trophical Index(ITI) was marked below 20 within 20 m distance from the edge of the Site A. The result of trap experiment, the solid deposition from the Site A was $34,485g\;m^{-2}yr^{-1}$ at 0 m from the center of the cage and $18,915g\;m^{-2}yr^{-1}$ at 42 m. From a model simulation, it was estimated that using a model simulation, the proportion of unfed food was $40\%$ at the Site A and the annual total amount of solid deposition was 63,401 accounting for $24.4\%$ of the annual total food fed at the Site A. The area solid deposition settled was estimated to be $8,450m^2$, which was about 16 times of the total area of fish cage at the Site A. And concerning ITI and abundance of benthos, the model predicted that sustainable solid flux at the Site A was below $10,000gm^{-2}yr^{-1}$. The percentage of food wasted was main element of solid deposition at the marine cage fish farms, and for minimizing solid deposition it is necessary to increase the efficiency of the food uptake. Based on the result of the model simulation, if the percentage of food wasted decreases to $10\%$ from the current $40\%$, then the solid deposition could decrease to a half. In addition, it was predicted that if farmers use EP pellets as food fed instead of MP and fish trash, solid deposition could decrease by $57\%$. Also this study proposes that the cage facility ratio of the licensed area be decreased to less than $5\%$ to minimize the sediment pollution.

• 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.