• Journal of Food Hygiene and Safety
• /
• v.38 no.3
• /
• pp.79-88
• /
• 2023

Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO₄ and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.

• The Korean Journal of Pesticide Science
• /
• v.15 no.2
• /
• pp.125-133
• /
• 2011

Ametryn is used in USA, China, and Japan, but not introduced in Korea yet. So, MRL (Maximum Residue Level), and analytical method of ametryn were not establishment in Korea. Therefore, this experiment was conducted to establish a determination method for ametryn residue in crops using HPLC-UVD/MS. Ametryn residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover ametryn from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The ametryn was quantitated by HPLC with UVD, using a Tosoh ODS 120T ($4.6{\times}250$ mm) column. The crops were fortified with ametryn at 2 levels per crop. Mean recovery ratio were ranged from 83.7% for a 0.2 mg/kg in soybean to 91.1% for a 1.0 mg/kg in hulled rice. The coefficients of variation were ranged from 1.2% for a 1.0 mg/kg in hulled rice to 3.6% for a 1.0 mg/kg in soybean. Quantitative limit of amatryn was 0.02 mg/kg in representative 5 crop samples. A LC/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 ametryne in agricultural commodities.

• Horticultural Science & Technology
• /
• v.34 no.1
• /
• pp.183-194
• /
• 2016

This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was $0.004mg{\cdot}kg^{-1}$ in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.

• Journal of Food Hygiene and Safety
• /
• v.8 no.3
• /
• pp.147-150
• /
• 1993

A novel rapid and sensitive method to detennine residual oxolinic acid in Acetes japonicus was developed. The residual oxolinic acid was extracted with ethylacetate and diluted oxalic acid, and interfering substances were removed by hexane. Fifty ppb residual concentration in the extract could be quantitated by UV-HPLC and the recovery rates were 79-91% according to the fortified amounts.

• Journal of Food Hygiene and Safety
• /
• v.7 no.1
• /
• pp.23-28
• /
• 1992

전남지방의 주요 재배단제에서 채취한 총 16종의 복숭아들에 대한 농약 잔류량 조사하였으며, 이들 복숭아를 수세 및 탈피 그리고 저장하였을 때의 농약 잔류량의 변화를 고찰하고자 하였다. 총 24종의 조사대상 농약중 TPN(Chlotothalonil) 및 Diazinon 그리고 Fenitrothion만이 3지점의 시료에서 검출되었으며 그 잔류량은 보사부에서 설정한 잔류허용기준(Maximum Residue Limits : MRL)에 크게 미달되는 수준이었다. 그러나 이들 시료들을 수세 및 탈피하지 않고 분석한 결과 TPN의 우 MRL을 훨씬 초과한 양이 검출되었는데, Diazinon은 MRL에는 미치니 못하였지만 수세 및 탈피한 시료들보다 높은 수준으로 검출되었다. 수세에 의한 복숭아중의 잔류농약의 경감효과는 TPN의 경우 63.4~66.4% 이었으며 Diazinon은 거의100% 수준이었다. 한편 탈피에 의한 잔류농약의 경감효과는 TPN 및 Diazinon 모두에서 대부분 제거되어 수세에 의한 경감보다도 훨씬 우수하다는 것을 알 수 있었다. 시료를 2주간 저장한 후 복숭아를 수세나 탈피를 하지 않거나 수세만 하여도 TPN과 Diazinon이 대부분 제거되며, 탈피를 한 경우는 별로 차이가 없었다.

• Journal of Food Hygiene and Safety
• /
• v.1 no.2
• /
• pp.163-169
• /
• 1986

소, 돼지, 닭 및 염소의 근육, 지방조직 및 내장부위에서 11가지 유기염소계 잔류농약을 분석하여 다음과 같은 결과를 얻었다. 1. 육류시료 모두에서 검출된 유기염소계의 잔류량은 $\alpha$-BHC, $eta$-BHC, pp'-DDE, Heptachlor epoxide, ${\gamma}$-BHC순으로 검출되었고, Heptachlor, pp'-DDE 및 pp'-DDD는 극미량 내지는 흔적 정도 검출되었고 Drins류는 검출되지 않았다. 2. Total BHC 잔류량의 범위는 소의 경우 0.389ppb~1.111ppb로 평균 0.713ppb였고, 돼지는 0.139ppb~0.150ppb로 평균 0.631ppb였으며 닭은 0.312ppb~0.80ppb로서 평균 0.517ppb였다. 그리고 염소의 경우에는 0.238ppb~1.134ppb로써 평균 0.586ppb의 수준이었다. 3. 육류별 잔류량은 소, 돼지, 염소, 닭의 순서이고 부위별 잔류량은 지방조직이 가장 많았고 그 다음이 근육, 그외 부위별 잔류량의 차이는 거의 없었다.

• Journal of Applied Biological Chemistry
• /
• v.63 no.3
• /
• pp.267-274
• /
• 2020

The dissipation characteristics and kinetics of fungicide mandipropamid and insecticide thiamethoxam in lettuce under greenhouse conditions were investigated at three different lettuce-growing fields for estimating the pre-harvest residue limits (PHRLs). The analytical methods were fully validated for the quantitation of pesticide residues using High-Performance Liquid Chromatography-Photo Diode Array detector or Ultraviolet-Visible Detector and applied to real samples. The lettuces suitable for shipment were harvested during 10 days including pre-harvest interval after treatment at the recommended dose by safe-use guidelines. The initial mean residues in different fields were 6.68-17.87 and 4.96-8.31 mg/kg for mandipropamid and thiamethoxam, respectively, which decreased to 16-54 and 14-44% in 10 days. The clothianidin, a metabolite of thiamethoxam, was detected in <0.02 to 0.37 mg/kg. The dissipation of both pesticides followed first-order kinetics over a period of 10 days after application. Based on the residue data, the mean dissipation rate constant (λ) and biological half-lives (T_1/2) were estimated to be -0.1060 and 6.5 days of mandipropamid and -0.1236 and 5.6 days of thiamethoxam. The PHRLs for lettuce on the 10th and 5th day before harvesting were calculated to be 63.24 and 43.56 mg/kg for mandipropamid, and 44.66 and 25.88 mg/kg for thiamethoxam, with -0.0746 and -0.1091 of the upper 95% confidence intervals of dissipation rate constant, respectively. This work would be useful as guidance for adjusting the shipment date and contribute to stabilizing the income of farmers in Korea.

• Proceedings of the Korean Environmental Sciences Society Conference
• /
• 2004.05a
• /
• pp.271-273
• /
• 2004

Enzyme inhibition기술을 이용한 습식 및 건식 kit는 carbmate계 농약의 잔류를 검출하는데 매우 민감하므로, carbmate계 잔류농약을 신속하게 검색할 수 있다. 즉 AChE효소를 이용한 습식 및 건식 kit로 carbamate계 농약을 검출 할 수 있다. 따라서 빠르고 간편하게 carbamate계 농약을 검출하기 위한 습식 kit 및 건식 kit로 상업화 할 수 있다.

• Proceedings of the KSAR Conference
• /
• 2002.06a
• /
• pp.180.2-181
• /
• 2002

• 한국환경농학회:학술대회논문집
• /
• 2009.04a
• /
• pp.105-115
• /
• 2009