• Journal of Applied Biological Chemistry
• /
• v.59 no.4
• /
• pp.331-336
• /
• 2016

Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.

• Journal of Applied Biological Chemistry
• /
• v.63 no.2
• /
• pp.153-159
• /
• 2020

The analytical method was established for simultaneous determination of fungicide prochloraz and its metabolites in several animal commodities using gas chromatography (GC) coupled with electron capture detector (ECD). Samples including beef meat, pork meat, chicken meat, milk, and egg were hydrolyzed with pyridine hydrochloride which converts prochloraz and its metabolites to 2,4,6-trichlorophenol (2,4,6-TCP) because residue definition for prochloraz was 'sum of prochloraz and its metabolites containing the 2,4,6-trichlorophenol moiety, expressed as prochloraz', for compliance with MRLs from animal commodities. Therefore, residual prochloraz was extracted with acetone, decomposed to 2,4,6-TCP, partitioned with dichloromethane, purified with aminopropyl SPE and quantified as 2,4,6-TCP with GC-ECD. The instrumental limit of quantitation and method LOQ (MLOQ) was 0.01 ㎍/mL and 0.02 mg/kg for prochloraz and 0.005 ㎍/mL and 0.01 mg/kg for 2,4,6-TCP, respectively. The linearity of the calibration curve was good with R² >0.995 in the range of 0.005-0.2 ㎍/mL. Fortification levels of prochloraz were 0.02 mg/kg (MLOQ) and 0.2 mg/kg (10MLOQ) for recovery tests. Overall recoveries of prochloraz were >90% with <10% of coefficient variation (C.V.). This established analytical method was fully validated and could be useful for quantification of prochloraz and its metabolites in animal commodities as official analytical method.

• Proceedings of the Korea Water Resources Association Conference
• /
• 2006.05a
• /
• pp.1431-1438
• /
• 2006

유역에서의 하천 프랙탈은 본 연구의 목적은 상수도 배수시스템의 수질예측 모형인 EPANET의 수질보정을 위한 염소분해계수의 효율적인 적용을 평가하기 위한 것이다. 이를 위해 우선적으로 연구대상시스템의 특성에 따른 수질 및 관종별 염소분해계수를 실험에 의하여 분석하고, 대상블록에 대한 EPANET 모형의 수질보정을 위한 잔류염소분해계수의 3가지 적용방법을 검토하여 효율적인 적용방안을 도출하였다. 연구결과, 실험에 의한 염소분해계수는 계절적 특성과 관종 및 관경에 따른 다양한 결과를 보였으며, 각 방법에 따른 모의결과도 다양하게 나타났으며, 관종, 관경, 계절적 특성을 반영한 분해계수를 적용한 모의 결과가 현장분석된 잔류염소농도와 더 가깝게 예측되는 것으로 나타났다. 따라서 EPANET을 이용하여 잔류염소농도를 예측하기 위해서는 대상수질 및 관망의 특성을 반영한 잔류염소분해계수를 사용하는 방법이 가장 효율적일 것으로 사료된다.

• The Korean Journal of Pesticide Science
• /
• v.15 no.4
• /
• pp.366-373
• /
• 2011

This study was conducted to identify the residue patterns of fungicide boscalid in ginseng cultivated for 4 or 6 years treated by various spraying methods. The pesticide was sprayed separately on ginseng according to safe use guideline, and the field was divided into three groups and they were traditional, soil and vinyl mulching applications. The maximum residue amounts of boscalid were 0.76 mg/kg in traditional application group, 0.69 mg/kg in soil application group, 0.62 mg/kg in vinyl mulching application group in the whole part of 4 years old ginseng, respectively. These residue levels in ginseng exceeded the maximum residue limit established by Korea Food & Drug Administration, which is 0.3 mg/kg.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2010.02a
• /
• pp.169-169
• /
• 2010

박막형 CIGS 태양전지의 배면전극으로 사용되는 Mo 박막은 낮은 저항으로 인한 전기전도성과 열적 안전성이 아주 우수하다. 연구에서는 연성 CIGS 태양전지의 제조를 위한 Mo 배면전극의 대면적 증착기술에 관한 것으로 DC Magnetron Sputtering 공정을 이용하여 전주기술을 통한 Ni-Fe계 연성기판재 위에 졸걸법으로 합성된 $SiO_2$ 절연박막에 Mo 박막을 증착하는 것을 목적으로 하고 있다. 실험에서는 연성기판재 대신 시편을 Sodalime glass, Si wafer, SUS계 소재를 사용하여 스퍼터링 공정에 의한 Mo 박막을 증착하였다. 실험에서 타겟에 인가되는 전력과 공정압력을 변수로 하여 Mo 박막의 증착율, 전기저항성을 측정하였다. 타겟의 크기는 $80mm{\times}350mm$, 타겟과 기판간 거리 20cm 이었으며, 공정 압력은 2~50 mtorr 영역에서 인가전력을 0.5-1.5kW로 하였다. Mo 박막의 증착율과 전기적 특성을 측정하기 위하여 $\alpha$-step과 4-point probe(CMT-SR 1000N)를 이용하였다. 그리고 Mo 박막의 잔류응력을 측정하기 위하여 잔류응력측정기를 이용하였다. Mo 박막의 미세구조분석을 위하여 SEM 및 XRD를 분석을 실시하였다. 배면전극으로서 전기저항성은 공정압력에 따라 좌우 되었으며, 2 mTorr 공정압력과 1.5kW의 전력에서 최소값인 $8.2\;{\mu}{\Omega}-cm$의 저항값과 증착율 약 $6\;{\mu}/h$를 보였다. 기판재와의 밀착성과 관련한 잔류응력 측정과 XRD분석을 통한 결정립 크기를 분석하여 공정압력에 따른 Mo 박막의 잔류응력과 전기 저항 및 결정립 크기의 상관관계를 조사하였다. 그리고 대면적 CIGS 증착공정을 위해 직각형 타겟을 통해 증착된 Mo 박막의 증착분포를 20cm 이내 조사하였다.

• The Korean Journal of Pesticide Science
• /
• v.19 no.3
• /
• pp.218-229
• /
• 2015

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On November 2012 the testing was carried out using the soil collected and kept as the moistened state for five years, which was expected to very low residue levels of pesticides. The soil was fortified with azoxystrobin, imidacloprid and methabenzthiazuron in a manner similar to prepare soil samples for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soils treated as different levels, one of which was used to the assessment and another used to confirm. In addition, provided three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty eight institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of azoxystrobin were 48, imidacloprid and methabenzthiazuron 46.

• The Korean Journal of Pesticide Science
• /
• v.17 no.2
• /
• pp.94-106
• /
• 2013

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

• Journal of Food Hygiene and Safety
• /
• v.34 no.3
• /
• pp.235-241
• /
• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.

• The Korean Journal of Pesticide Science
• /
• v.19 no.3
• /
• pp.195-203
• /
• 2015

Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

• The Korean Journal of Pesticide Science
• /
• v.18 no.4
• /
• pp.321-329
• /
• 2014

This experiment was conducted to establish an analytical method for residues of amisulbrom, as recently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops using HPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was diluted with 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives and sensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible and easy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.