• 한국환경농학회지
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• 제39권3호
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• 한국환경농학회지
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• 제21권2호
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• pp.149-155
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• 2002

상추의 생산단계에서의 잔류허용기준 설정과 최종 소비단계에서의 안전성 평가자료로 활용하기 위하여 지금까지 상추수확물에서의 잔류수준과 검출빈도가 높은 것으로 알려진 살충제 chlorpyrifos 및 살균제 procymidone의 포장상태에서의 생물학적 반감기, 보관상태에 따른 잔류량 변화 그리고 세척형태에 따른 제거율을 조사하였다. 시설재배포장에서 상추중두 약제의 살포농도별 생물학적 반감기를 측정한 결과 기준량 살포의 경우 chlorpyrifos 1.2일 및 procymidone 1.3일 배량살포의 경우에는 chlorpyrifos 1.5일 및 procymidone 2.6일로 나타났다. 유통과정중에서 일어날 수 있는 두 가지 농약의 잔류량 변화를 알아보기 위해서 실온(20$^{\circ}C$) 및 냉장(4$^{\circ}C$) 상태로 보관하면서 두 약제의 잔류량 변화를 조사한 결과 반감기는 실온저장시 chlorpyrifos 3.8일, procymidone 20.9일이었고, 냉장저장시에는 chlorpyrifos 12.4일 procymidone 20.9일로 나타나 두 약제 모두 실온저장보다 냉장저장시 잔류량의 감소가 훨씬 느린 것으로 나타났다. 세척방법에 의한 잔류농약의 감소량을 조사한 결과 세제 사용시의 평균 제거율은 chlorpyrifos 48.3%, procymidone 52.6%로 나타났고, 물 사용 시에는 chlorpyrifos 31.3%, procymidone 38.1%로 나타났다.

• Journal of Biosystems Engineering
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• 제30권2호
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• pp.114-120
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• 2005

In this study, a biological reaction and measurement control system was developed to rapidly measure the insecticide imidacloprid residues in agricultural products. The biological reaction part of the system was designed to include micro-pumps and valves for fluid transport, and a polystyrene covet as a reaction chamber. The measurement control part of the system consisted of a photodiode with a light-emitting diode for optical density measurement, and a control microcomputer to implement assay. Signal output was read as the rate of change in optical density at 645 nm. The sensitivity of the system was 2.2 ng/mL ($IC_50$). The system could execute a measurement cycle in about 19 minutes. Research will be continued to develop an automatic sampler fur imidacloprid residues from agricultural products.

• 한국식품위생안전성학회지
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• 제20권3호
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• pp.165-174
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• 2005

This survey was conducted to monitor the current status of pesticide residues in agricultural products collected in wholesale markets and big retailers in Gwangju, in 2004. A total of 751 samples was analyzed by multiresidue method. Vegetables and fruits accounted for the largest proportion of the commodities analyzed and those two commodity groups comprised 604 $(80\%)\;and\;83\;(11\%)$ of the total number of 751 samples. Of these 751 samples, 112 samples $(14.9\%)$ had pesticide residues and 29 samples $(3.9\%)$ had violative residues. The detection rate was the highest $25\%$ in January and the lowest $9.5\%$ in June. The violation rate was the highest $7.0\%$ in March and the lowest $0\%$ in April. The violation rate in wholesale products was higher than that in big retailer products, $5.8\%$ verses $3.5\%$. And of 112 samples with pesticide residues, the agricultural product in which the pesticide residues were the most flequently detected was perilla leaf $(17.9\%)$ followed by korean lettuce $(16.1\%)$, spinach $(8.0\%)$ and korean cabbage $(5.4\%)$ and among 112 samples, 22 samples $(20\%)$ had more than one pesticide. Procymidone $(20.3\%)$, endosulfan $(18.2\%)$, dimethomorph $(13.3\%)$, chlorpyrifos $(7.7\%)$ and azoxystrobin $(6.3\%)$ were the most frequently found in agricultural product analyzed.

• 분석과학
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• 제34권1호
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• pp.1-8
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• 2021

An analytical method was developed and optimized for the quantification of a plant growth regulator, 2,6-diisopropylnaphthalene (2,6-DIPN), in agricultural products using gas chromatography-tandem mass spectrometry. The samples were extracted, partitioned, and were purified using a Florisil® cartridge. To validate the analytical method, its specificity, linearity, limit of detection (LOD) and limit of quantification (LOQ) of the instrument, LOQ of the analytical method (MLOQ), accuracy, and repeatability were considered. The method displayed excellent results during validation, and is suitable for the determination and quantification of the low residual levels of the analyte in the agricultural samples. All of the results with the optimized method were satisfactory and within the criteria ranges requested in the Codex Alimentarius Commission guidelines and the Ministry of Food and Drug Safety guidelines for pesticide residue analysis. The developed method is simple and accurate and can be used as a basis for safety management of 2,6-DIPN.

• 농약과학회지
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• 제14권2호
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• pp.86-94
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• 2010

본 연구는 2006년 3월부터 2008년 12월까지 부산지역 농산물도매시장으로 유입되는 경매 전 농산물 7,237건에 대해 다종농약다성분법으로 잔류농약검사를 실시하였다. 이 중 1,164건 (16.1%)에서 농약이 검출되었으며, 231건 (3.2%)은 잔류허용기준을 초과하였다. 기준초과된 농산물은 대부분 해당 농산물에 대한 잔류허용기준이 정해져 있지 않아서 잠정기준을 적용받는 경우로서 기준초과된 231건 중 181건으로 78.4%가 이에 해당한다. 농약성분별로 endosulfan, procymidone, chlorothalonil, ethoprophos, chlorpyrifos, diethofencarb, kresoxim-methyl, EPN 순으로 잔류허용기준이 초과되었다. 잔류농약이 검출된 1,164건의 농산물 중 211건에서 두 종류 이상 농약이 검출되었고 이 중 37.9%에 해당되는 80건이 기준초과되었다. 본 연구에서 농약 잔류허용기준을 초과하는 요인은 해당 농산물에 대한 미적용 농약의 사용, 두 종류 이상의 농약사용으로 나타났다.

• 한국정밀공학회:학술대회논문집
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• 한국정밀공학회 2008년도 추계학술대회 논문집
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• pp.365-366
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• 2008

• 한국환경농학회지
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• 제39권2호
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• pp.130-137
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• 2020

BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r²>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

• 분석과학
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• 제26권2호
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• pp.154-163
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• 2013

국내 신규 제초제로 등록된 pyrimisulfan에 대해 농산물 중 잔류실태를 조사하기 위하여 LC-MS/MS를 이용한 시험법을 개발하였다. Pyrimisulfan 시험법의 회수율은 현미, 감자, 감귤, 고추에서 0.005 mg/kg 수준에서 88.7~99.3%이고 0.05 mg/kg수준에서 각각 90.1~94.2%였다. 회수율에 대한 모든 분석오차는 10% 미만으로 Codex 잔류물질 분석 가이드라인에 만족하였다.16 분석을 위한 기기 조건에서 pyrimisulfan의 정량한계는 0.005 mg/kg이었으며 0.01~1.0 mg/kg 범위에서 상관계수(R) 0.999 이상의 높은 직선성을 보여주었다. 따라서 본 연구에서 개발된 잔류농약 시험법은 농산물을 대상으로 효과적인 시료 전처리 방법과 최적의 정제 과정을 확립하여 다양한 농산물에 대한 잔류량 검출이 적당함을 확인할 수 있었다. 이와 같이 확립한 pyrimisulfan의 잔류시험법은 국제적 분석 기준을 만족할 뿐만 아니라 분석과정의 신뢰성 또한 확보할 수 있어서 본 잔류농약 시험법은 공정시험법으로 사용 될 것이다.

• 혜화의학회지
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• 제22권1호
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• pp.129-143
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• 2013

This study was conducted to investigate the residue amount of pesticide on the 41 medicinal herbs in Daejeon area. This study was carried out to monitor the current status of pesticide residues in commercial medicinal herbs for sale of food use in 2012. It was performed using GC/ECD, GC/NPD, HPLC to analyze pesticides residues. Residues of 283 pesticides were analyzed by a simultaneous multiresidue method in 41 medicinal herbs being on sale in Daejeon. The medicinal herbs detected pesticides in 10 of 41 cases, showed a detection rate of 24.39%. The medicinal herbs which exceed the maximum residue limit were five cases as Cnidii Rhizoma, Osterici Radix, Artemisiae Capillaris Herba, Zizyphi Fructus and Alismatis Rhizoma. And pesticide residue of Cnidii Rhizoma and Alismatis Rhizoma exceeds the limit standard presented in only medicine use of KFDA. The residual pesticides which had the high detection rate were Chlopyrifos, Tebuconazole and Endosulfan in the detection of medicinal herbs. For further research, standards of Pesticide Residues in medicinal herbs should be added and more research of pesticide residues in medicinal herbs required. And standards of pesticide residues in medicinal herbs should be applied equally as medicines and food.