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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.
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.
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.
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.
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 ),황정인 ( Jeong-in Hwang ),이상협 ( Sang-hyeob Lee ),강민수 ( Min-su Kang ),정혜현 ( Hye-hyun Jung ),류준상 ( Jun-sang Ryu ),홍성현 ( Sung-hyun Hong ),곽세연 ( Se-yeon Kwak ),강자군 ( Ja-gun Kang ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 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 선행연구에서 개발된 Korea Pesticide Residue Analysis-Positive List System (KOPRA-PLS)방법을 적용하여, 적합한 PLS 체계용 고감도 신속 잔류 다종농약다성분 분석법을 개발하고자 한다. 분석대상 농약은 식품공전 다종농약다성분 분석법-제 1법에 등록된 농약 및 국내 미등록 농약 중 liquid chromatography-tandem mass spectrometry (LC-MS/MS)로 분석 가능한 농약인 61종을 선정하였으며, 대표시료는 현미를 선정하여 사용하였다. KOPRA-PLS 방법에서 추출 및 액액분배 방법은 균질화된 시료를 acetonitrile로 첨가하여 homogenizer로 추출 후, sodium citrate, sodium chloride 및 anhydrous sodium sulfate를 첨가하여 액액분배하였다. 정제방법은 primary secondary amine 및 anhydrous magnesium sulfate를 첨가하여 dispersive solid phase extraction 방법으로 정제하였다. LC-MS/MS로 분석 가능한 61종 농약에 대한 validation test를 실시한 결과, 분석대상농약의 정량한계는 모두 0.01 mg/kg 이하로 나타났으며, matrix-matched standard calibration의 상관계수가 모두 0.99 이상으로 나타나 직선성이 양호한 것으로 나타났다. LC-MS/MS로 분석 가능한 61종 농약중에서 52종의 농약이 회수율 70∼120%, 변이계수 20% 이하를 만족하였다. 따라서 본 시험에 의해 확립된 52종의 농약은 screening method로 사용하기에 적절한 것으로 판단되었으며, 추후PLS체계를 위한 다성분분석법 연구가 지속적으로 수행되어야 할 것으로 생각된다.