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엇갈이 배추의 배춧국 가공시 Triazole계 살균제의 분해양상
류준상 ( Jun-sang Ryu ),이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kwak ),홍성현 ( Seong-hyun Hong ),강자군 ( Ja-gun Kang ),김장억 ( Jang-eok Kim ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
This study was carried out to calculate the processing factors of triazole fungicides on cabbage soup made in Korean cabbage. Hexaconazole and myclobutanil were sprayed 3 times at interval of 7 days prior to harvest day on Korean cabbage. Harvested Korean cabbage was parboiled in boiling water for 30 secs and boiled for 10 and 30 mins with ingredients. Residue amounts of the pesticides in raw and processed products of Korean cabbage were analyzed using a GC-ECD. Their initial residues in Korean cabbage were 1.51 mg/kg for hexaconazole and 3.44 mg/kg for myclobutanil. The residue amounts of hexaconazole and myclobutanil in Korean cabbages were dissipated by up to 80.63% and 46.03%, respectively, through parboiling. During boiling for cabbage soup, dissipation rates of hexaconazole were 93.13-96.25% and myclobutanil were 66.41-70.26%, respectively. Processing factors of pesticides in processed Korean cabbage were calculated 0.21-0.04 for hexaconazole and 0.57-0.31 for myclobutanil, respectively. When processing factor is low, the residue amounts has been more removed compared with the initial residues. This results indicated that dissipation rates of hexaconazole is higher than myclobutanil during cabbage soup processing, there are many environmental factors affecting residue amounts. Overall, processing of cabbage soup could be give a significant dissipation effect above 70.26% on tested triazole pesticides in Korean cabbage.
엇갈이 배추 가공 과정 중 Hexaconazole 및 Myclobutanil 살균제의 잔류량 변화
류준상(Jun-Sang Ryu),이상협(Sang-Hyeob Lee),곽세연(Se-Yeon Kwak),강자군(Ja-Gun Kang),홍성현(Sung-Hyeon Hong),황정인(Jeong-In Hwang),김장억(Jang-Eok Kim) 한국농약과학회 2017 농약과학회지 Vol.21 No.4
Triazole fungicides, hexaconazole and myclobutanil, were sprayed on Korean cabbage to calculate the processing factors using their residue amounts during Kimchi and cabbage soup processing. Recoveries rates of hexaconazole and myclobutanil in Korean cabbage were 88.7-95.7% and 81.6-98.4%, respectively. Their initial residues in Korean cabbage were 1.51 mg/kg for hexaconazole and 3.44 mg/kg for myclobutanil. The residue amounts of hexaconazole, during Kimchi processing, further dissipated by 67.6% in washing process, 68.9-74.8% in brining process and 78.8-94.0% during fermentation. Those of myclobutanil further dissipated by 45.6% in washing process, 51.5-61.6% in brining process and 55.2-76.7% during fermentation. During cabbage soup processing, the residue amounts of hexaconazole further dissipated by 79.5% in parboiling process, 92.7-93.4% in soakaging process and 92.7-96.0% in boiling process. Those of myclobutanil further dissipated by 43.0% in parboiling process, 44.2-47.1% in soakaging process and 64.5-68.6% in boiling process. Compared with the initial residue in Korean cabbage, hexaconazole and myclobutanil were dissipated by 94.0-96.0% and 68.6-76.7%, respectively, during Kimchi and cabbage soup processing. The processing factors of hexaconazole during Kimchi and cabbage soup processing were 0.06-0.32 and 0.04-0.21, respectively, and those of myclobutanil were 0.23-0.54 and 0.31-0.57, respectively. Overall, various processing process to Kimchi and cabbage soup can give a significant dissipation effect on tested triazole pesticides in Korean cabbage.
LC-MS/MS를 이용한 잔류농약 다성분 분석법의 Matrix Effect 비교
이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kawk ),류준상 ( Jun-sang Ryu ),강자군 ( Ja-gun Kang ),홍성현 ( Sung-hyun Hong ),도정아 ( Jung-ah Do ),장문익 ( Moon-ick Jang ),이규식 ( Gyu-seek Rhee ),이영득 ( Young-deuk Lee ),김장억 ( 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
This study was conducted to compare with the multi-residue analysis method for reduced a matrix effect in three agricultural products, such as orange, green pepper and brown rice. QuEChERS method involves single-phase extraction of 10 g sample with 10 mL acetonitrile. On the other hand, the improved method extracted 10 g of sample with 50 mL acetonitrile. Clean-up step used in the QuEChERS method was the d-SPE using PSA, but C18 of SPE cartridge was used for the improved method. As a result, both methods were similar in linearity and limit of quantification. The ratios that satisfy the Codex guideline were 85% of total pesticides for AOAC QuEChERS method and 88% for the improved method. Matrix effects showed different results, however, the improved method was found to produce least matrix effect. Average matrix effect QuEChERS method was -38%, and those of the improved method was -10%. Comparison of matrix effects for different agricultural products showed high variability for some residues such as dimethylthiocarbamate. It was indicated that the amount of co-extracting compounds that cause ionization suppression of pesticides depends on the agricultural products as well as on the sample preparation method employed. As a conclusion, the improved method appears to be a more suitable method because it can reduce the matrix effect rather than the QuEChERS method.
Liquid Chromatography-Tandem Mass Spectrometry를 이용한 농산물 중 살충제 다성분 동시분석법
이상협 ( Sang-hyeob Lee ),황정인 ( Jeong-in Hwang ),강민수 ( Min-su Kang ),정혜현 ( Hye-hyun Jung ),류준상 ( Jun-sang Ryu ),홍성현 ( Sung-hyun Hong ),곽세연 ( Se-yeon Kwak ),강자군 ( Ja-gun Kang ),도정아 ( Jung-ah Do ),장문익 ( Mo 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
For regulating pesticide residues in agricultural products imported from other countries, Korea is ready to introduce the Positive List System permitting the determination of unregistered pesticides in them at a concentration of <0.01 mg/kg. Hence, it is required to establish a rapid and sensitive analysis method for both registered and unregistered pesticides in imported agricultural products, in order to ensure their safety from pesticide residues. In this study, we developed an analytical method for 62 insecticides in three agricultural products such as orange, green pepper, and brown rice using liquid chromatography-tandem mass spectrometry. Acetonitrile and sodium citrate were used for the extraction of insecticide residues from the samples, and a dispersive solid phase extraction using primary secondary amine and anhydrous magnesium sulfate was employed for a clean-up. Using the developed method, the limits of quantification were below 0.01 mg/kg for all tested insecticides, and their matrix-matched standard calibration curve had high correlation coefficients of >0.99. In addition, for all tested samples, recoveries of insecticides fortified at levels of 0.01-0.05 mg/kg ranged from 75.2 to 111.3%, and relative standard deviations were acceptable at <18.1%. Therefore, the analytical method developed in this study could be used as the rapid and sensitive analysis method for 62 insecticides in agricultural products.
인삼의 생육 및 가공에 따른 살균제 Propamocarb의 잔류특성
이용재(Yong-Jae Lee),류준상(Jun-Sang Ryu),김성수(Seong-Soo Kim),서현석(Hyun-Seok Seo),나은식(Eun-shic Na),이민정(Min-Jeong Lee),홍성수(Sung-Soo Hong),서수경(Su-Gyeong Seo),권혜영(Hye-Young Kwon) 한국농약과학회 2020 농약과학회지 Vol.24 No.2
This study was carried out to elucidate residual characteristics of propamocarb in ginseng and calculate its processing factors in processed products, such as dried ginseng and red ginseng. Propamocarb 50% SC (Suspension Concentrate) was diluted at 1,000 times and applied 4 times onto ginseng with a 10-day interval, according to its pre-harvest interval (PHI). Limit of quantitation (LOQ) in fresh ginseng and its processed products were 0.01 ㎎/㎏. Recoveries of the analytical methods in fresh ginseng and its processed products ranged from 74.8 to 89.6%. Concentration of propamocarb in fresh ginseng ranged from < 0.01 ㎎/㎏ to 0.042 ㎎/㎏ and in dried ginseng ranged from < 0.01 ㎎/㎏ to 0.033 ㎎/㎏. The residual amounts of propamocarb in red ginseng was from 0.053 to 0.107 ㎎/㎏. The maximum residual amount at 0, 7, 14, 21, 30 and 50 day after last application was 0.102 ㎎/㎏. Processing factors of propamocarb were 0.8 in dried ginseng and 2.0, 2.5 in red ginseng.
토양 중 살충제 Dinotefuran과 대사체의 분해양상
곽세연 ( Se-yeon Kwak ),이상협 ( Sang-hyeob Lee ),류준상 ( Jun-sang Ryu ),홍성현 ( Seong-hyeon Hong ),강자군 ( Ja-gun Kang ),김장억 ( Jang-eok Kim ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
This study was performed to investigate microbial degradation patterns of dinotefuran(DIN) and its metabolites(DN, UF and MNG) in soils under laboratory conditions based on result of field trials. In the field trials, DIN was treated with concentration of 2 mg/kg on the radish cultivated and non-cultivated soil before seeding radish. The initial residue amounts of DIN was 2.01 mg/kg and decreased to below limit of quantitaion (LOQ) at 60 days after treatement which result in the formation of UF upto 0.21 mg/kg for radish cultivated soils. While initial residues of DIN in non-cultivated soils was 2.00 mg/kg and steadily decreased 84% with 0.32 mg/kg at 70 day. UF as well as DN were produced after 50 days in non-cultivated soil. DIN was spiked with 2 mg/kg in each of 20 g sterilized and unsterilized soil and analysed at 0, 1, 3, 7, 14, 21, 30, 45 and 60 day after treatment under laboratory conditions. The residue amounts of DIN at 0 days were 1.97 mg/kg for sterilized soil and 1.99 mg/kg for unsterilized soil and both of them were decreased with a similar decline curve by 45 and 54% at end of experiment day, respectively. The degradation rate of DIN in unsterilized soil was higher than that of sterilized soil, which means mircroorganism was one of the factors that affected the degradation of DIN in soils. As the degradation of DIN by microorganisms in unsterilized soil, DN and UF were detected respectively upto 0.01 and 0.03 mg/kg and MNG was not detect.
고감도 신속 다종농약다성분 검색/검사법 개발 연구 - LC-MS/MS법
김장억 ( Jang-eok Kim ),이상협 ( Sang-hyeob Lee ),곽세연 ( Se-yeon Kwak ),류준상 ( Jun-sang Ryu ),홍성현 ( Sung-hyun Hong ),강자군 ( Ja-gun Kang ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-
현재 우리나라는 세계 여러 나라와 자유무역협정(FTA: Free Trade Agreement)을 체결하여 수입농산물이 지속적으로 증가하고 있다. 이에 따라, 우리나라는 자국 농산물 및 소비자를 보호하기 위하여 자국기준이 설정되지 않은 농약들에 대하여 0.01 mg/kg 이상 잔류하는 농산물에 대해 규제를 하는 Positive List System (PLS)의 도입이 시급하다. 따라서 PLS 체계 운용 시 잔류최소기준을 실질적으로 적용할 수 있는 국가 공정잔류분석법의 확립이 필수적으로 요구된다. 본 연구는 다종농약다성분 분석법-제2법을 LC-MS/MS 대상성분 115종에 대하여 적용하여 분석법을 검증하고자 한다. 시료는 오렌지를 사용하였으며, 유지 농산물 분석을 위한 탈지과정을 추가한 시험법은 대두 시료를 사용하였다. 다종농약다성분 분석법-제2법에 명시된 시료량 및 추출용매량을 조절하여 시료량 10 g 및 추출용매량 20 mL로 진행하였으며, 이에 따라 시험방법을 비율에 따라 조절하였다. 115종 농약에 대한 validation test를 실시한 결과, 분석대상농약의 정량한계는 모두 0.01 mg/kg 이 하로 나타났으며, matrix-matched standard calibration의 상관계수가 오렌지의 경우 0.8972-1.000으로 나타났으며, 대두는 0.9103-0.9995로 나타났다. 다성분 분석법 기준인 70∼120%, 변이계수 20% 이하의 회수율 시험을 만족하는 농약의 수는 오렌지 105성분, 대두 97성분 이었다. 따라서 본 시험에 의해 확립된 115종의 농약은 screening method로 사용하기에 적절한 것으로 판단되었으며, 추후PLS체계를 위한 다성분분석법 연구가 지속적으로 수행되어야 할 것으로 생각된다.
살충제 Dinotefuran의 무에 대한 흡수이행 및 잔류 양상
곽세연(Se-Yeon Kwak),황정인(Jeong-In Hwang),이상협(Sang-Hyeob Lee),강민수(Min-Su Kang),류준상(Jun-Sang Ryu),강자군(Ja-Gun Kang),홍성현(Sung-Hyeon Hong),유오종(Oh-Jong You),김장억(Jang-Eok Kim) 한국농약과학회 2017 농약과학회지 Vol.21 No.3
The residual amounts of dinotefuran (DIN) applied to cultivated soil and radish leaf were investigated to assess uptake and residual patterns of DIN through the root and leaf. Recoveries for residual analysis of pesticides spiked with two different concentration on the radish root, leaf and soils were 85.5-104.9%. The degradation half-life of DIN in soils treated with 2.01 and 9.35 mg/kg of initial residues were 6.2-8.9 days and showed rapid degradation patterns. When analyzed radish harvested every 10 days from 40 to 70 days which were cultivated in DIN treated soil, the uptake rates from soil to whole radish by root were 4.9 to 16.7%. Root uptake amounts of DIN were 0.020-0.057 mg/kg for low (2.01 mg/kg) treatment and 0.066-0.256 mg/kg for high (9.35 mg/kg) treatment, respectively. Absorbed DIN were more distributed in the leaf than root at the early stage of harvesting, but the distribution of DIN in root tended to increase as time passage. On the other hand, as a result of foliar spraying with the standard amount, 2 times and 5 times according to the safe use standard of DIN, the initial residual amounts of DIN in leaf were 0.397, 0.788 and 1.172 mg/kg for each treatment level. And leaf uptake rates from leaf to root during experimental period were 1.7 to 7.1%. These results will be useful for determining management criteria for soil persisted pesticides.
살균제 Fludioxonil 및 Metconazole의 밀 부위별 잔류 양상
강자군 ( Ja-gun Kang ),황정인 ( Jeong-in Hwang ),이상협 ( Sang-hyeob Lee ),강민수 ( Min-su Kang ),정혜현 ( Hye-hyun Jung ),곽세연 ( Se-yeon Kwak ),류준상 ( Jun-sang Ryu ),홍성현 ( Seong-hyeon Hong ),박준홍 ( Jun-hong Park ),김장억 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-
Residual patterns of fungicides fludioxonil and metconazole applied on wheat with their safe use guidelines were investigated with consideration for their distribution rates in each compartment of wheat. The fungicides were 2 or 3 times sprayed on wheats at the interval of 7 days prior to harvest. Wheat samples collected at final harvest day were divided into three compartments such as grain, hull and straw, and the pesticide residue analysis was individually carried out to such compartments of wheat. The analytical methods of fungicide residues in wheat were acceptable, with recoveries of 84.3 to 113.3% and correlation coefficients of 0.1 to 4.7%. Due to the systemic characteristics, the residual amounts of metconazole in the grain part of wheat were greater as 0.11~0.29 mg/kg than those amounts (0.02~0.07 mg/kg) for fludioxonil, and these residual amounts of both fungicides exceeded their maximum residue limits. According to absolute residue amounts of the fungicides in one wheat plant, their distribution rates in each compartment of wheat were the highest in straws (66.7~70.7%), followed by hulls (29.0~32.5%) and grains (0.2~0.9%). Although the distribution rates of fludioxonil and metconazole in wheat were the lowest in the edible grain parts, their high distribution rates in hulls and straws, available as feeds for livestock, may result in safety problems by pesticide residues. Therefore, it is required to assess the residual characteristics of pesticides in individual compartments of crops in order to ensure the safety for either foods to human or feeds to livestock from their residues.