• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.63-68
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• 2013

Ethyl carbamate (EC) is a contaminant generated in the fermentation processes of various fermented foods. In this study, residue levels of EC in 95 alcoholic beverage samples were determined by using Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS). All the samples were purified by a liquid-liquid extraction (LLE) method using dichloromethane. The LLE method enables an improvement in time and cost to detection and specificity over the conventional extraction methods. The limits of detection and quantification (LOD and LOQ) to analyze EC were 1.3 and 4.0 ng/mL, respectively. The recovery rates of EC were ranged from 90.0 to 97.5% at the levels of 50, 100, and 500 ug/L. Among traditional grain-based alcoholic beverage samples (n = 34), the average residue levels of EC in takju, yakju, and cheongju were 0.63, 7.01, and 14.11 ug/L, respectively. Among fruit-based alcoholic beverage samples (n = 48), those of EC in japanese apricot spirits, bokbunjaju, grape wines, and other fruit wines were 79.18, 1.66, 2.64, and 2.39 ug/L, respectively. Among distilled or diluted alcoholic beverage samples (n = 13), those of EC in soju (distilled or diluted), general distillates, liquors, and brandies were 0, 3.30, 8.20, and 8.52 ug/L, respectively. Therefore, this study reports that the residue levels of EC in the alcoholic beverages, distributed in the current domestic markets, did not reach its maximum allowed levels of 30 and 400 ug/L established for grape and fruit wines in Canada, respectively.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.68-74
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• 2017

An analytical method for detecting metamifop residue in paddy water, soil, and rice with high performance liquid chromatography (HPLC) was developed. Water was extracted with ethyl acetate before analyzing by HPLC. Soil residues were extracted with acetone under acidic condition and after purifying with $Extrelut^{(R)}$ NT, and silica SPE, the residue was analyzed by HPLC. For residue analysis in rice, the procedure involved extraction with acetone, purification with $Extrelut^{(R)}$ NT, partitioning between acetonitrile/hexane, purification with silica SPE cartridge, and analysis by HPLC. The limit of detection (LOD) was 1.0 ng, limit of quantitation (LOQ) was 3.0 ng, and method limit of quantitation (MLOQ) were 0.001 mg/L for paddy water, 0.01 mg/kg for rice and soil, respectively. Standard calibration curve shows linearity from 0.05 mg/kg to 5.0 mg/kg ($R^2=0.9999$). The recoveries in fortified paddy water were $91.3{\pm}3.5%$ (0.01 mg/L level) and $93.2{\pm}6.3%$ (0.05 mg/L level). The recoveries in fortified paddy soils were $92.5{\pm}4.0%$ (0.1 mg/kg level) and $92.7{\pm}4.0%$ (0.5 mg/kg level) in soil A, while, $102.3{\pm}4.4%$ (0.1 mg/kg level) and $98.9{\pm}7.9%$ (0.5 mg/kg level) in soil B, respectively. The recoveries in fortified rice were $93.0{\pm}6.9%$ (0.1 mg/kg level) and $85.0{\pm}3.5%$ (0.5 mg/kg level). This method was proved to be effective and can be used to determine the metamifop residue in paddy water, paddy soil, and rice.

• 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.

• Korean Journal of Environmental Agriculture
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• v.14 no.1
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• pp.23-27
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• 1995

The cross-reactivities of antibody derived from rabbit immunized with metalaxyl-HSA conjugate were identified to 44% and 28% for metalaxyl acid and metolachlor respectively. The detection range of metalaxyl in competitive ELISA was 5 ppb to 5 ppm. The recoveries of metalaxyl in ELISA for 6 crops; potato, sesame, pepper, cabbage, cucumber and onion was ranged 77.5-103.6%. In this test, CV% were calculated below 10% except for sesame sample as shown 21.5%.

• Analytical Science and Technology
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• v.15 no.1
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• pp.67-71
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• 2002

The residual analysis and half-life time of imidazole fungicide prochloraz in soils (silty clay) were investigated by gas chromatography equipped electron capture detector (GC-ECD). The soil samples were extracted acetone/hexane(1:1) solvent and analyzed after separated by $LC-NH_2$ Sep-Pak solid column. Linear sensitivity of standard calibration curve was Y = 268.8600X + 0.0664, $R^2=0.9998$ between 0.05~1.00 ng. The detection limit was 0.02 mg/L and the average recoveries were 94.5~97.3% from the standard additional experiments with 0.10 and 0.40 mg/L. The half-life time was 24.4 days in room laboratory and 7.6 days in the field test soil.

• Transactions of the Korean Society of Automotive Engineers
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• v.15 no.1
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• pp.1-7
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• 2007

In this study, the influence of compressive residual stress and corrosive condition for corrosion fatigue crack was investigated, after immersing in 3.5%NaCl, $10%HNO_3+3%HF,\;6%FeCl_3$. The immersion period was performed for 90days. The fatigue characterization of a spring steel with processed shot peening were performed by considering the several corrosion environments in the range of stress ratio of 0.05 by means of opening mode displacement. By using the methods mentioned above, the following conclusions have been drawn: The fatigue life shows more improvement in the shot peened material than that in the un peened material. And the fatigue life shows improvement in ambient than in corrosion conditions. Threshold stress intensity factor range of the shot peened materials has higher than of the un peened materials. And the threshold stress intensity factor range was decreased in corrosion environments over ambient.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2015.05a
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• pp.28-28
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• 2015

현재 인쇄전자 소자 생산을 위해 사용되고 있는 대부분의 그라비아 롤러는 미세 패턴의 보호와 인쇄 중 마찰에 대한 내구성을 향상시키기 위해 경질 크롬 도금 막이 사용되고 있다. 그러나 경질 크롬 도금 막의 경우 구현할 수 있는 경도(~1000 HV)와 이형성, 내마찰(마찰계수: ~ 0.6) 특성 등에 한계가 있다. 이러한 경질 크롬 도금이 적용된 그라비아 롤은 그 수명과 내구성, 구현할 수 있는 인쇄 품질 및 신뢰성 그리고 인쇄처리 속도 등에 있어 여러 문제가 있다. DLC(Diamond Like amorphous Carbon)는 낮은 마찰계수 값인 0.2 이하와 뛰어난 내마모성, 상대재료에 대한 이형성 등을 겸비한 표면강화 기술로 경질 크롬 도금막 대비 우수한 표면 경도(>1,800 HV) 특성을 갖으며, 합성된 DLC 코팅 막의 경우 정밀 인쇄 제판이 요구하는 표면거칠기를 구현할 가능성이 높다는 장점이 있다. 특히 실리콘이 첨가 된 Si-DLC의 경우 표면의 마찰계수를 0.1 이하까지 낮출 수 있는데 닥터블레이드 및 잉크, 인쇄 기재와의 마찰 훼손을 최소화시켜 그라비아 인쇄 롤의 수명을 향상시킬 수 있다. 또한 PECVD 공정을 이용하여 합성한 Si-DLC는 표면거칠기를 10nm 이하의 경면으로 구현할 수 있으며, 높은 접촉각에 의한 우수한 이형성을 통해 미세 패턴 내부에 전자잉크/페이스트가 잔류되는 현상을 억제할 수 있다. 이는 기존 경질 크롬 도금이 적용된 그라비아 롤에서 발생하는 패턴 내 잉크 잔류-고형화와 그에 의한 사용수명 단축현상을 현저히 개선시킬 수 있다.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.307-313
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• 2013

This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.123-129
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• 2014

The present work was aimed to determine the pre-harvest residue limits (PHRLs) and the safety management of commonly used pesticides namely buprofezin and penthiopyrad on oriental melon (Cucumis melon var. makuwa). In this study, the buprofezin (diluted two thousand fold) and penthiopyrad (diluted four thousand fold) were sprayed single time on oriental melon in the cultivation areas Sangju (site 1) and Sungju (site 2). Oriental melon were randomly collected from the both areas at the end of 0 (2 hours after pesticides spaying), 1, 2, 3, 5, 7, 9 and 10 days. For analysis, each samples were partitioned twice (80 and 70 mL) with dichloromethane and purified by florisil SPE cartridge. Finally, the residual amounts of both pesticides in all samples were analyzed using gas chromatography/nitrogen phosphorus detector (GC/NPD). In this study, the method limit of quantification (MLOQ) for both buprofezin and penthiopyrad in oriental melon was found to be $0.01mg\;kg^{-1}$ and their recovery levels were 91.1~98.6% and 90.0~104.6%, respectively. Further, the calculated biological half-life for buprofezin and penthiopyrad in oriental melon were 3.9 and 3.5, and 3.0 and 2.7 days in site 1 and 2, respectively. The results of this study found that the PHRLs for buprofezin and penthiopyrad were 4.24 and $2.31mg\;kg^{-1}$, respectively at 10 days before harvest. Consequently, the present study suggest that the residual amounts of both pesticides will be lower than the maximum residue limits (MRLs) when oriental melon is harvested.

• Korean Journal of Environmental Agriculture
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• v.18 no.4
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• pp.384-387
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• 1999

The residue of imidacloprid in hulled rice and paddy soil was investigated. In laboratory conditions, the degradation of imidacloprid in the soils followed first-order reaction kinetic. The rate of degradation was influenced by soil temperature and soil type. The half-life of imidacloprid at $18-28^{\circ}C$ was 66.7-96.3 days in the heavy clay soil and 56.8-117.5 days in the clay loam soil. Arrhenius activation energy obtained from the temperature experiment was 25.5 KJ/mol in heavy clay soil and 50.3 KJ/mol in clay loam soil. In paddy field, the degradation of imidacloprid was fast during the initial period but the degradation rate was gradually slow. About 10 % of the initial amount remained in the soil 120 day after the application. The residual amount of imidacloprid in rice was below the detection limit, 0.01 ppm. The residue level in rice was lower than MRL 0.05ppm in Korea.