• Title/Summary/Keyword: residual range

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A Safety Survey on Pesticide Residues in Dried Agricultural Products (건조농산물의 잔류농약 안전성 조사)

  • Lee, Hyo-Kyung;Oh, Moon-Seog;Jeong, Jin-A;Kim, Ki-Yu;Lee, Seong-Bong;Kim, Han-Taek;Kang, Hyang-Ri;Son, Ji-Hee;Lee, Yun-Mi;Lee, Mi-Kyoung;Lee, Byoung-Hoon;Kim, Ji-Won;Park, Yong-Bae
    • Journal of Food Hygiene and Safety
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    • v.34 no.4
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    • pp.340-347
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    • 2019
  • We performed a safety survey on residual pesticides in dried agricultural products. A total of 110 samples of dried agricultural products distributed in Gyeonggi-do were analyzed for 263 pesticides according to multi class pesiticide multiresidue method. Ten types of pesticides were detected in 10 samples. Chlorpyrifos was detected in Ricinus communis leaves, chlorpyrifos, hexaconazole, pyridalyl in Chwinamul (wild aster), diniconazole, isoprothiolane, lufenuron in radish leaves, hexaconazole in Cirsium setidens (Korean thistle), bifenthrin, and chlorothalonil, boscalid, and pyraclostrobin in pepper leaves. The detection rate of pesticides was 9.1%, and among these samples, one was detected over Maximum Residue Limits (MRLs). In the validation study, the values of limit of detection (LOD), limit of quantitation (LOQ), coefficient of determination ($R^2$) and recovery were in the range of 0.002~0.027 mg/kg, 0.006~0.083 mg/kg, 0.9964~1.0000 and 74.8~118.9%, respectively. The Positive List System (PLS) was newly introduced as part of the safety management of residual pesticide in agricultural products in Korea in 2019. With the application of the PLS, if the MRL is not established, 0.01 mg/kg limit is applied uniformly. In spite, these of strengthened residue limits, the MRLs of dried agricultural products are still insufficient. Therefore, this study could be utilized as basic data for the setting of proper MRLs.

Determination and Validation of an Analytical Method for Dichlobentiazox in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Choi, Ha Na;Yoon, Sang Soon;Jung, Young-Hyun;Yoon, Hae Jung
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.108-117
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    • 2021
  • BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C18 showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Determination and Validation of an Analytical Method for Spiropidion and Its Metabolite Spiropidion-enol (SYN547305) in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Spiropidion 및 대사산물 Spiropidion-enol (SYN547305) 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Lee, Jung Mi;Jung, Yong-hyun;Moon, Guiim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.82-94
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    • 2022
  • BACKGROUND: Spiropidion and its metabolite are tetramic acid insecticide and require the establishment of an official analysis method for the safety management because they are newly registered in Korea. Therefore, this study was to determine the analysis method of residual spiropidion and its metabolite for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods (original, AOAC, and EN method) were applied to optimize the extraction method, and the EN method was finally selected by comparing the recovery test and matrix effect results. Various adsorbent agents were applied to establish the clean up method. As a result, the recovery of spiropidion was reduced when using the dispersive-SPE method with MgSO4, primary secondary amine (PSA), graphitized carbon black (GCB) and octadecyl (C18) in soybean. Color interference was minimized by selecting the case including GCB and C18 in addition to MgSO4. This method was established as the final analysis method. LC-MS/MS was used for the analysis by considering the selectivity and sensitivity of the target pesticide and the analysis was performed in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 79.4-108.4%, with relative standard deviation and coefficient of variation were less than 7.2% and 14.4%, respectively. CONCLUSION(S): Spiropidion and its metabolite could be analyzed with a modified QuEChERS method, and the established method would be widely available to ensure the safety of residual insecticides in Korea.

Monitoring of Residual Pesticides and Exposure Assessment of Olive Oil Products Sold on the Market (올리브유의 잔류농약 모니터링 및 노출량 조사)

  • Mi-Hui Son;Jae-Kwan Kim;You-Jin Lee;Ji-Eun Kim;Eun-Jin Baek;Byeong-Tae Kim;Seong-Nam Lee;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.4
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    • pp.211-216
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    • 2023
  • A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R2) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

Selection and Validation of an Analytical Method for Trifludimoxazin in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Trifludimoxazin의 시험법 선정 및 검증)

  • Sun Young Gu;Su Jung Lee;So eun Lee;Chae Young Park;Jung Mi Lee;Inju Park;Yun Mi Chung;Gui Hyun Jang;Guiim Moon
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.79-88
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    • 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.

Classification of Transport Vehicle Noise Events in Magnetotelluric Time Series Data in an Urban area Using Random Forest Techniques (Random Forest 기법을 이용한 도심지 MT 시계열 자료의 차량 잡음 분류)

  • Kwon, Hyoung-Seok;Ryu, Kyeongho;Sim, Ickhyeon;Lee, Choon-Ki;Oh, Seokhoon
    • Geophysics and Geophysical Exploration
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    • v.23 no.4
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    • pp.230-242
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    • 2020
  • We performed a magnetotelluric (MT) survey to delineate the geological structures below the depth of 20 km in the Gyeongju area where an earthquake with a magnitude of 5.8 occurred in September 2016. The measured MT data were severely distorted by electrical noise caused by subways, power lines, factories, houses, and farmlands, and by vehicle noise from passing trains and large trucks. Using machine-learning methods, we classified the MT time series data obtained near the railway and highway into two groups according to the inclusion of traffic noise. We applied three schemes, stochastic gradient descent, support vector machine, and random forest, to the time series data for the highspeed train noise. We formulated three datasets, Hx, Hy, and Hx & Hy, for the time series data of the large truck noise and applied the random forest method to each dataset. To evaluate the effect of removing the traffic noise, we compared the time series data, amplitude spectra, and apparent resistivity curves before and after removing the traffic noise from the time series data. We also examined the frequency range affected by traffic noise and whether artifact noise occurred during the traffic noise removal process as a result of the residual difference.

Uncertainty of Agrometeorological Advisories Caused by the Spatiotemporally Averaged Climate References (시공간평균 기준기후에 기인한 농업기상특보의 불확실성)

  • Kim, Dae-jun;Kim, Jin-Hee;Kim, Soo-Ock
    • Korean Journal of Agricultural and Forest Meteorology
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    • v.19 no.3
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    • pp.120-129
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    • 2017
  • Agrometeorological advisories for farms and orchards are issued when daily weather exceeds a predefined range of the local reference climate, which is a long-term average of daily weather for the location. The reference climate at local scales is prepared by various simplification methods, resulting in uncertainty in the agrometeorological advisories. We restored daily weather data for the 1981-2010 period and analyzed the differences in prediction results of weather risk by comparing with the temporal and spatial simplified normal climate values. For this purpose, we selected the agricultural drought index (ADI) among various disaster related indices because ADI requires many kinds of weather data to calculate it. Ten rural counties within the Seomjin River Basin were selected for this study. The normal value of 'temporal simplification' was calculated by using the daily average value for 30 years (1981-2010). The normal value of 'spatial simplification' is the zonal average of the temporally simplified normal values falling within a standard watershed. For residual moisture index, temporal simplification normal values were overestimated, whereas spatial simplification normal values were underestimated in comparison with non-simplified normal values. The ADI's calculated from January to July 2017 showed a significant deviation in terms of the extent of drought depending on the normal values used. Through this study, we confirmed that the result of weather risk calculation using normal climatic values from 'simplified' methods can affect reliability of the agrometeorological advisories.

Characteristics of Heavy Metals (Ba, Cr) Distribution in Soil (토양 중 중금속(Ba, Cr)의 분포특성 평가)

  • Yoon, Jeong-Ki;Kim, Rog-Young;Kim, Ji In;Noh, Hoe-Jung;Yu, Soon-Ju;Kim, Tae Seung;Lee, Myung Gyu;Yun, Dae-Geun;Lee, Hong-gil;Kim, In Ja;Park, Gyoung-Hun
    • Journal of Soil and Groundwater Environment
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    • v.20 no.7
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    • pp.61-69
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    • 2015
  • This study was performed to provide fundamental data to establish the new soil pollution standards and the soil contamination management plans in a rational manner. The distribution characteristics of new soil contaminants such as barium (Ba) and chromium (Cr) in soils (n=140) were investigated in relation to land-use classification and geological features. Also, the sequential extraction test was conducted to evaluate fate and mobility of new soil contaminants. The soil samples taken from 140 sites were analyzed to survey distribution levels of selected new soil contaminants. The average concentration and range for hazardous metals (Ba, Cr) were Ba 128.946 (26.757~489.587) mg/kg, Cr 30.121 (2.579~132.783) mg/kg. Based on land use classification, the highest Ba concentration was found in factory soils, followed by dry field and park soils, while Cr concentration was highest in rice paddy soils, followed by dry field and factory soils. Within 10 geological units investigated the highest Ba and Cr concentrations were observed in the soils from Okcheon group and metamorphic rocks, respectively. The BCR (European Community Bureau of Reference) sequential extraction was conducted to identify chemical distributional existence of 2 elements of soils from each geological unit. Ba in soils is mainly assumed to exists as reducible form (such as BaSO4, BaCO3) and Cr in soils mainly is assumed to exist as residual form (such as Cr2O3, CrxFe1-x(OH)3(x < 1)).

Changes in the Concentrations of the Tap Water Chlorination By-Products by Heating during Cooking, and Human Ingestion Exposure (조리시 가열에 따른 수돗물 중 염소소독부산물의 농도 변화와 인체 섭취 노출)

  • 김희갑;이수형
    • Environmental Analysis Health and Toxicology
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    • v.14 no.1_2
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    • pp.35-43
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    • 1999
  • A number of disinfection by-products (DBPs) are formed as a result of the addition of chlorine into the public water supply and some of them have been suggested to cause adverse health effects on humans. However, the estimation of human ingestion exposure to each DBP has been performed simply by multiplying the concentration of a chemical in the cold tap water by the volume of water consumed during a given period of time. However, a questionnaire concerning water consumptions administered to sixty people residing in Chunchon showed that the volume of tap water consumed accounted for approximately 70% of the total volume of water consumed and that of heated water represented approximately 94% of tap water ingested. Heating durations for water-containing foods (e. g., soups and pot stews) and heated beverages (e. g., barley tea) were grouped into 10, 20, 30, and 35 minutes. Based on these time frames, an aluminum pot containing one liter of tap water was heated for the above respective time periods using a gas range to determine the variations of the concentrations of individual DBPs by heating. The pH and total residual chlorine were measured before and after heating. Collected water samples were carried to the laboratory and analyzed for eight DBPs and total organic carbon. Chloroform, bromodichloromethane, chloral hydrate, 1, 2-dichloro-2-propanone, 1, 1, 1-trichloropropanone, and dichloroacetonitrile were not detected following heating for 10 minutes and longer. The concentration of dichloroacetic acid (DCAA) was elevated with heating duration, resulting in the averages of 2.0, 3.1, 4.7, and 12 times the initial concentration, respectively, for 10, 20, 30, and 35 minute heating periods. On the other hand, the concentration of trichloroacetic acid (TCAA) decreased with heating duration, with 0.65, 0.40, 0.34, and 0.19 times lower than the initial concentration. Therefore, it is suggested that ingestion exposure to DCAA increases with heating duration but that ingestion exposure to TCAA decreases. In addition, while the amount of DCAA was elevated at the initial time periods (10 or 20 minutes) and then slowly decreased, that of TCAA was rapidly decreased. In conclusion, water-heating processes during cooking influence the concentrations of individual DBPs in the tap water, with lower levels for volatile DBPs and TCAA, and higher levels for DCAA. Therefore, concentration change needs to be taken into consideration in the estimation of human ingestion exposure to DBPs.

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