시설재배 딸기의 생산단계에서 살충제 잔류량에 따른 반감기 및 감소상수 산출에 의한 안전성 평가 Residue Dissipation Kinetics and Safety Evaluation of Insecticides on Strawberry for the Harvest Periods in Plastic-covered Greenhouse Conditions원문보기
BACKGROUND: Dissipation patterns of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry grown in plastic-covered greenhouse were evaluated at 7 intervals including the preharvest interval after application. This study was performed to determine the re...
BACKGROUND: Dissipation patterns of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry grown in plastic-covered greenhouse were evaluated at 7 intervals including the preharvest interval after application. This study was performed to determine the residue concentrations, half-lives and dissipation rates in strawberry for the harvest periods. METHODS AND RESULTS: Acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam were applied in accordance with critical good agricultural practices for strawberry. Strawberry samples were collected at 0, 1, 2, 3, 5, 7 and 10 days after application. Quantitaion was performed by HPLC/DAD and HPLC-MSMS system with C18 column. The limit of quantitation (LOQ) values varied between were 0.00025~0.05 mg/kg on strawberry. The recoveries of acequinocyl, clothianidin, diflubenzuron, thiacloprid and thiamethoxam at two concentrations ranged from 70.9~104.9% on strawberry. The half-lives of pesticide dissipation on strawberry for two fields ranged from 1.3~8.2 days. The dissipation rates were evaluated according to the statistics method with a 95% confidence. CONCLUSION: The residue levels of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry at 0-day after application were below the specified values by Korean MRL. To estimate dissipation rate constant of pesticides on crop for harvest periods, it is important to set the pre-harvest residue limit for human health and consumer protection in Korea.
BACKGROUND: Dissipation patterns of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry grown in plastic-covered greenhouse were evaluated at 7 intervals including the preharvest interval after application. This study was performed to determine the residue concentrations, half-lives and dissipation rates in strawberry for the harvest periods. METHODS AND RESULTS: Acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam were applied in accordance with critical good agricultural practices for strawberry. Strawberry samples were collected at 0, 1, 2, 3, 5, 7 and 10 days after application. Quantitaion was performed by HPLC/DAD and HPLC-MSMS system with C18 column. The limit of quantitation (LOQ) values varied between were 0.00025~0.05 mg/kg on strawberry. The recoveries of acequinocyl, clothianidin, diflubenzuron, thiacloprid and thiamethoxam at two concentrations ranged from 70.9~104.9% on strawberry. The half-lives of pesticide dissipation on strawberry for two fields ranged from 1.3~8.2 days. The dissipation rates were evaluated according to the statistics method with a 95% confidence. CONCLUSION: The residue levels of insecticides (acequinocyl, clothianidin, diflubenzuron, thiacloprid, and thiamethoxam) on strawberry at 0-day after application were below the specified values by Korean MRL. To estimate dissipation rate constant of pesticides on crop for harvest periods, it is important to set the pre-harvest residue limit for human health and consumer protection in Korea.
본 연구는 딸기에 등록되어 사용되고 있는 농약 중 생산단계 잔류허용기준이 설정되어 있지 않은 살충제 5종(acequinocyl, clothianidin, diflubenzuron, thiacloprid, thiamethoxam)을 농약안전사용 기준에 따라 약제를 살포하고 농약의 일자별 잔류특성으로부터 감소상수 및 반감기를 산출하여, 생산단계 농약잔류허용기준 설정을 위한 기초자료로 활용하므로서, 생산단계에서부터 잔류농약을 관리하여 유통단계 농산물의 안전성 확보에 기여하고자 한다.
제안 방법
농약 잔류량 확인을 위한 시료채취는 약제처리 후 0, 1, 2, 3, 5, 7 및 10일차에 출하시기에 적합한 크기로 선정하여 1 kg이상이 되도록 채취하였다. 채취한 시료는 시험농약 및 시료채 취일자를 기재한 polyethylene bag에 넣어, 24시간 이내에 실험실로 운반하였다.
분석법 정량한계(Limit of Quantitation, LOQ)는 표준용 액을 이용하여, 기기분석 크로마토그램에서 Signal to noise ratio(S/N)가 10 이상을 최소 검출량으로 하여 시료무게(g), 기기 주입량(μL), 분석용액의 최종부피(mL) 및 희석배수를 적용하여 산출하였다[5].
회수율 시험농도는 모든 시험농약의 정량한계, 정량한계 10배 및 50배 수준에서 잔류량 확인이 가능하도록 2개 이상의 농도를 선정하여, 무처리시료에 표준용액을 처리하여 3반복 시험을 수행하였다. Acequinocyl은 회수율 시험을 위하여 조제한 시료 20 g에 acetone 100 mL를 가하여 250 rpm으로 20분간 교반 한 후 추출물은 여과지(Whatman Grade 6, 110 mm)로 감압⋅여과한 후, rotary vacuum evaporator (EYELA rotary evaporator N-1110 Series)를 이용하여 40℃에서 감압 농축하였다.
대상 데이터
시험포장은 시설재배의 2개의 지역을 선정하여, acequinocyl, diflubenzuron, thiacloprid, clothianidin은 논산시(포장 I, 품종: 설향)와 예산군(포장 II, 품종: 설향), Thiamethoxam 은 논산시(포장 I, 품종: 설향), 홍성군(포장 II, 품종: 설향)에서 수행하였고, 위도상의 거리차이는 각각 약 56 km 및 46 km였다.
딸기 중 acequinocyl, clothianidin, diflubenzuron, thiacloprid 및 thiamethoxam의 일자별 잔류량을 적용하여 회귀분석에 의해 감소상수 및 생물학적 반감기를 산출하였으며, F-검정 및 t-검정을 수행하여 회귀방정식 및 감소상수의 유의성을 확인한 후, 95% 신뢰수준의 감소상수 하한값과 반감기를 산출하였다(MFDS, 2014).
성능/효과
본 연구에서는 처리한 시험약제는 딸기에 등록된 농약제품중 유효성분함량이 높고, 최종약제살포 후 수확일이 짧아 잔류 가능성이 높은 안전사용기준(Critical Good Agricultural Practice, cGAP)에 해당하는 제품을 선정하여 살포하였고, 살포 후 0일차에 채취한 시료의 잔류량은 소비자의 안전성에 근거하여 설정된 농약별 잔류허용기준의 4.5∼70%로 낮은 수준 이었으며, 소비자가 유통단계에서 섭취할 수 있는 딸기에 해당 되는 최종살포 후 수확일의 평균 농약잔류량은 농약별 잔류허 용기준의 1.1∼36%로 소비자에게 안전한 수준이었다. 미국 농무부(U.
시설재배 딸기에서 시간경과에 따른 잔류량으로 부터 통계 학적 방법에 의한 회귀분석을 수행하여 시험포장 1, 2의 감소상수(95% confidence level)의 하한값은 acequinocyl 0.1196과 0.0885, clothianidin 0.0516과 0.0610, diflubenzuron 0.2577과 0.3634, thiacloprid 0.0875와 0.0655, thiamethoxam 0.0714 및 0.0578이었고, 생물학적 반감기는 acequinocyl 4.4 일과 6.4일, clothianidin 8.3일과 9.0일, diflubenzuron 1.4일과 1.3일, thiacloprid 6.4일과 7.7일, thiamethoxam 7.1일과 7.6일로 시험포장에 따른 반감기가 유사하였다(Table 2). 이전의 연구에서 시험농약의 농산물 중 반감기가 acequinocyl은깻잎에서 2.
시설재배조건에서 생산단계 딸기에 시험약제 acequinocyl, clothianidin, diflubenzuron, thiacloprid 및 thiamethoxam 를 처리한 후 채취한 0일차 시료의 잔류량은 acequinocyl 0.31~0.72 mg/kg, clothianidin 0.025~0.034 mg/kg, diflubenzuron 0.07~0.11 mg/kg, thiacloprid 0.34~0.78 mg/kg, thiamethoxam 0.14~0.23 mg/kg이었고, 각각의 시험농약에 대한 딸기 중 잔류허용기준은 1.0, 0.5, 2.0, 2.0 및 1.0 mg/kg으로 모든 농약이 약제처리 후 0일차에 잔류허 용기준 이하로 잔류하였다(Table 1, Fig. 1).
후속연구
본 연구는 국내에서 딸기에 등록되어 사용되고 있는 농약에 대한 생산단계에서의 일자별 잔류량 및 감소경향예측을 통하여 유통단계에서 농약잔류허용기준을 초과하는 부적 합율을 감소시켜, 생산자에게 경제적 손실을 최소화하고, 소비자의 안전성 확보를 위한 기초자료로 활용할 수 있다.
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