• Title/Summary/Keyword: QuEChERS

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Development of Simultaneous Analytical Method for Thiodicarb and its Metabolite Methomyl in Livestock Products (축산물 중 Thiodicarb와 대사산물 Methomyl의 동시분석법개발)

  • Chang, Hee-Ra;You, Jung-Sun;Ban, Sun-Woo;Gwak, Hye-min
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.142-147
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    • 2021
  • BACKGROUND: Agricultural use and pest control purposes of pesticides may lead to livestock products contamination. Thiodicarb and its degraded product, methomyl, are carbamate insecticides that protect soya bean, maize, fruit, and vegetables and control flies in animal and poultry farms. For maximum residue limit enforcement and monitoring, the JMPR residue definition of thiodicarb in animal products is the sum of thiodicarb and methomyl, expressed as methomyl. This residue definition was set to consider the fact that thiodicarb was readily degraded to methomyl in animal commodities. And therefore the simultaneous analytical method of thiodicarb and methomyl is required for monitoring in livestock products. METHODS AND RESULTS: The study was conducted using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and HPLC-MS/MS to determine the thiodicarb and methomyl in livestock products. The limit of quantitation (LOQ) was 0.01 mg/kg for livestock products, including beef, pork, chicken, milk, and egg. The coefficient of determinations (r2) for the calibration curve were > 0.99, which was acceptable values for linearity. Average recoveries at spiked levels (LOQ, 10LOQ, and 50LOQ, n=5) in triplicate ranged from 73.2% to 102.1% and relative standard deviations (RSDs) were less than 10% in all matrices. CONCLUSION: The analytical method was validated for the performance parameters (specificity, linearity, accuracy, and precision) in livestock products to be acceptable by the CODEX guidelines.

Plant Back Interval of Fluopyram Based on Primary Crop-derived Soil and Bare Soil Residues for Rotational Cultivation of Radish (Fluopyram의 전작물 유래 및 나지조건 토양잔류성에 기초한 알타리무의 식물식재후방기간)

  • Kim, Young Eun;Yoon, Ji Hyun;Lim, Da Jung;Kim, Seon Wook;Cho, Hyunjeong;Shin, Byeung Gon;Kim, Hyo Young;Kim, In Seon
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.99-107
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    • 2021
  • BACKGROUND: Pesticide uptake by a rotational crop after being used for the primary crop is a potential cause of violation against the pesticide law if the pesticide is not registered in the secondary crop. This study was conducted to investigate the plant back interval (PBI) of fluopyram for the rotational cultivation of radish. METHODS AND RESULTS: Two experimental approaches were performed the evaluation of residues in radish cultivated successively in soil 16 days after treated with fluopyram onto pepper plant (T1) and in radish cultivated in bare soil treated with fluopyram at PBI 30 and PBI 60 days (T2). A modified QuEChERS method coupled with LC/MS/MS analysis showed good linearity of matrix-matched standard calibration of fluopyram with the coefficient values of determination greater than 0.995. Recovery values at levels of 0.01, 0.05, 0.1 and 0.25 mg/kg ranged from average 84.9 to 117.6% with RSD less than 10%. Fluopyram residues in radish harvested from T1 and T2 were found as levels less than maximum residue limit. CONCLUSION: This study suggests 20~30 days as the PBI of fluopyram for the rotational cultivation of radish in the greenhouse soil treated with fluopyram used for pepper as the primary crop.

Evaluation and application of pretreatment methods for pharmaceuticals and personal care products in the solid phase of sewage samples (하수처리시설 고상시료 중 잔류의약물질 분석을 위한 전처리법 평가 및 적용)

  • Park, Junwon;Kim, Changsoo;Ju, Byoungkyu;Lee, Wonseok;Chung, Hyenmi;Jeong, Dong-Hwan
    • Journal of Korean Society of Water and Wastewater
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    • v.32 no.6
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    • pp.559-572
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    • 2018
  • The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

Residue Characteristics and Risk Assessment of Pesticides (Boscalid and Pyraclostrobin) in Hylomecon vernalis (피나물 중 boscalid 및 pyraclostrobin의 토양 처리시 잔류특성 및 안전성 평가)

  • Yu, Ji-Woo;Song, Min-Ho;Kim, Jinchan;Lee, Kwanghun;Ko, Rakdo;Keum, Young-Soo;Lee, Jiho
    • Korean Journal of Environmental Agriculture
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    • v.41 no.2
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    • pp.95-100
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    • 2022
  • BACKGROUND: This study was aimed to determine characteristics of residues of the soil-treated boscalid and pyraclostrobin within Hylomecon vernalis and to evaluate the risks from intake of the residual pesticides in the crop. METHODS AND RESULTS: The pesticides were treated to soils at two different concentrations, and the plant samples were collected 57 days after seeding. The samples were extracted using the QuEChERS extraction kit (MgSO4 4 g, NaCl 1 g). The quantitative methods for boscalid and pyraclostrobin were validated using linearity, recovery, and CV (coefficient of variation). Risk assessment of the pesticides was performed using Korea national nutrition statistics 2019. CONCLUSION(S): The residual levels of boscalid were 0.02-0.05 mg/kg (for the treatment at 6 Kg/10a) and 0.05-0.08 mg/kg (for the treatment at 12 Kg/10a), respectively. The residual concentrations of pyraclostrobin were below the LOQ. The amounts of pesticides were less than Maximum Residue Limits specified by the Korean Ministry of Food and Drug Safety. The maximum hazard indices of boscalid in chwinamul and amaranth for consumers were 0.0075% and 0.1525%, respectively, and it indicates that the risk of the pesticides from the crop is considered to be low.

Assessing the Formation of Polycyclic Aromatic Hydrocarbons in Grilled Beef Steak and Beef Patty with Different Charcoals by the Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) Method with Gas Chromatography-Mass Spectrometry

  • Ali Samet Babaoglu
    • Food Science of Animal Resources
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    • v.43 no.5
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    • pp.826-839
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    • 2023
  • This study investigated the effects of different charcoals on the occurrence of 16 polycyclic aromatic hydrocarbons (PAHs) in grilled beef steaks and beef patties. Seven different charcoals were used as follows: from oak wood (C1), from orange wood (C2), from Valonia oak wood (C3), from Marabu wood (C4), extruded charcoal from beech wood (C5), from coconut shells (C6), and from hazelnut shells (C7). The grilling times for each charcoal type were 6 min for the beef patties and 7 min for the beef steaks, until the internal temperature reached at least 74℃. The total concentration of 16 PAHs (PAH16) in beef steaks grilled with C1 (35.75 ㎍/kg) and C7 (36.39 ㎍/kg) was higher than that of C3 (23.80 ㎍/kg) and C6 (24.48 ㎍/kg; p<0.05). The highest amounts of PAH16 (216.40 ㎍/kg) were determined in the beef patty samples grilled using C5 (p<0.05). The summation of benzo[a]anthracene, chrysene, benzo[b]fluoranthene and benzo[a]pyrene, referred to as PAH4, was not detected in any of the beef steaks, whereas it was determined in the beef patties grilled with C2 (7.72 ㎍/kg) and C5 (22.95 ㎍/kg; p<0.05). The PAH16 concentrations of the beef patty samples in each charcoal group were significantly higher compared to the beef steaks (p<0.05). To avoid the formation of high PAH levels, the use of extruded charcoal and hazelnut shell charcoal should therefore be avoided when charcoal grilling beef steaks and beef patties, and low-fat meat products should be preferred.

Residue Monitoring and Dietary Risk Evaluation of Fungicide Propiconazole in Leafy Vegetables under Greenhouse Conditions

  • Lawal Abdulkareem;Ji-Eun Oh;Se-Yeon Kwak;Sang-Hyeob Lee;Jae-Won Choi;Aniruddha Sarker;Kee Sung Kyung;Tae Hwa Kim;Jang-Eok Kim
    • Korean Journal of Environmental Agriculture
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    • v.42 no.3
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    • pp.193-202
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    • 2023
  • Residue monitoring of propiconazole (PCZ) in cabbage, shallot, and spinach was conducted under multi-trial greenhouse conditions. This study aimed to understand the fate of the applied fungicide in these vegetables. Furthermore, the associated health risk of PCZ in leafy vegetables was assessed through dietary risk assessment. Commercially available PCZ (22% suspension concentrate) was administered thrice according to the OECD fungicide application interval guideline. The plant samples were extracted using a slightly modified QuEChERS technique and analyzed using gas chromatography-tandem mass spectrometry. The average PCZ recovery was between 84.5% and 117.6%, with a <5% coefficient of variance. The dissipation of PCZ residue in cabbage, shallot, and spinach after 14 days was 96%, 90%, and 99%, respectively, with half-lives of <5 days. Meanwhile, dietary risk assessments of PCZ residues in the studied vegetables using the risk quotient (RQ) were significant < 100 (RQ < 100). Thus, the population groups considered in this study were not at substantial risk from consuming leafy vegetables sprayed with PCZ following critical, good agricultural practices.

Study on Residual Properties and Risk Assessment of α-Cypermethrin and Deltamethrin in the Chives (Allium tuberosum R.) and Spring onion (Allium wakegi Araki) (시설재배 부추(Allium tuberosum R.)와 쪽파(Allium wakegi Araki) 중 α-Cypermethrin과 Deltamethrin의 잔류특성 및 안전성 평가)

  • Jo, Yeong Ju;Choi, Jeong Yoon;Ham, Hun Ju;Hur, Jang Hyun
    • Korean Journal of Environmental Agriculture
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    • v.41 no.1
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    • pp.55-64
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    • 2022
  • BACKGROUND: This study was conducted to evaluate the residual characteristics and safety assessment of αcypermethrin and deltamethrin in minor crops, chives and spring onion cultivated in greenhouse. METHODS AND RESULTS: The insecticides α-cypermethrin 2% EC and deltamethrin 1% EC used in the experiment were diluted 1,000 times and then sprayed on chives and spring onion twice with 1-week intervals at 0, 7, 14, and 21 days before harvest. The residual insecticides were extracted from the minor crops using QuEchERS method and analyzed by GC-MS/MS. The average initial residues of α-cypermethrin and deltamethrin in chives after 21 days decreased from 2.74 to 0.82 mg/kg and 1.12 to 0.16 mg/kg, respectively. Similarly, in spring onion the residues after the same periods decreased from 0.26 to <0.01 mg/kg for α-cypermethrin and from 0.07 to <0.01 mg/kg for deltamethrin. CONCLUSION(S): The PHIs (pre-harvest intervals) for α-cypermethrin and deltamethrin in chives are recommended as 14 days before harvest with twice applications of the pesticides, whereas for α-cypermethrin in spring onion PHI of 7 days before harvest is recommended with 3 times of applications and PHI of 21 days for deltamethrin. The theoretical maximum daily intakes of cypermethrin and deltamethrin were 68.8% and 64.2%, respectively, indicating that residues of both compounds did not pose considerable health risks to consumers.

Evaluation of Residues of Fungicide Azoxystrobin in Radish based on Plant Back Interval Experiment (식물후방식재기간(PBI) 시험에 기반한 살균제 Azoxystrobin의 알타리무 중 잔류량 평가)

  • Yoon, Ji Hyun;Lim, Da Jung;Kim, Seon Wook;Kim, In Seon
    • Korean Journal of Environmental Agriculture
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    • v.41 no.1
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    • pp.1-8
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    • 2022
  • BACKGROUND: The pesticide residue in rotational crop is one of the main concerns to agricultural products because it has the potentiality of violating positive list system (PLS). Thus, the crops used for the rotational cultivation should be considered the pesticide residue patterns to meet the PLS guideline. In this study, we evaluated the residue patterns of fungicide azoxystrobin in radish based on plant back interval (PBI) experiment. METHODS AND RESULTS: Azoxystrobin was treated onto greenhouse soil at 217 g a.i./10a in two different regions. Radishes were sown onto the soil 30 and 60 days after azoxystrobin treatment. The soil and plant samples were subjected to a modified QuEChERS method and LC/MS/MS analyses to determine the residues of azoxystrobin. The methods were validated to meet the guidelines of the pesticide residue analysis recommended by the Rural Development Administration, Republic of Korea. Azoxystrobin was dissipated significantly in soil during the experimental period and found as a level less than 0.01 mg/kg in radish 30 and 60 days after treatment. Azoxystrobin residues in radish samples were lower than the maximum residue limit (MRL) for root vegetables. CONCLUSION(S): This study suggests 30 days as a PBI for rotational cultivation of radish in greenhouse soil that had been treated with azoxystrobin at a level of 217 g a.i./10a.

Establishment of Pre-Harvest Residue Limit (PHRL) of Fungicides Azoxystrobin and Difenoconazole on Prunus mume fruits (매실 중 살균제 azoxystrobin과 difenoconazole의 생산단계 잔류허용기준 설정)

  • Lee, Dong Yeol;Kim, Yeong Jin;Park, Min Ho;Lee, Seung Hwa;Kim, Sang Gon;Kang, Nam Jun;Kang, Kyu Young
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.307-313
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    • 2013
  • This study was carried out to investigate the residual characteristics of fungicide azoxystrobin and difenoconazole in Prunus mume fruits, and establish pre-harvest residue limits (PHRL) based on dissipation and biological half-lives of fungicide residues. The fungicides were sprayed onto the crop at recommended dosage once and 3 times in 7 days interval, respectively. The samples were harvested at 0, 1, 2, 4, 6, 8, 10, 12 and 14 days after treatment. These residual pesticides were extracted with QuEChERS method, clean-up with $NH_2$ SPE cartridge, and residues were analyzed by HPLC/DAD and GLC/ECD, respectively. Method quantitative limits (MQL) of azoxystrobin were 0.03 mg $kg^{-1}$ and of difenoconazole were 0.006 mg $kg^{-1}$. Average recovery were $93.2{\pm}2.49%$, $85.5{\pm}1.97%$ for azoxystrobin at fortification levels at 0.3 and 1.5 mg $kg^{-1}$, and $100.8{\pm}6.74%$, $87.6{\pm}9.92%$ for difenoconazole at fortification levels at 0.06 and 0.3 mg $kg^{-1}$, respectively. The biological half-lives of azoxystrobin were 5.9 and 5.2 days at recommended dosage once and 3 times in 7 days interval, respectively. The biological half-lives of difenoconazole were 9.3 and 8.0 days at recommended dosage once and 3 times in 7 days interval, respectively. The PHRL of azoxystrobin and difenoconazole were recommended as 5.32 and 1.64 mg $kg^{-1}$ for 10 days before harvest, respectively.

Development of Multi-residue Analysis and Monitoring of Persistent Organic Pollutants (POPs) - Used Organochlorine Pesticides in Korea (국내에 사용되어 금지된 유기염소계 농약류의 다중분석법과 모니터링)

  • Lim, Sung-Jin;Oh, Young-Tak;Yang, Ji-Yeon;Ro, Jin-Ho;Choi, Geun-Hyoung;Ryu, Song-Hee;Moon, Byeong-Chul;Park, Byung-Jun
    • The Korean Journal of Pesticide Science
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    • v.20 no.4
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    • pp.319-325
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    • 2016
  • This study was conducted to investigate residual organochlorine pesticides in green house soil and oriental melon, green pepper, and lettuce. The majority of them were designated as persistent organic pollutants (POPs) by the international community at the Stockholm Convention on Persistent Organic Pollutant. Extraction and clean-up method were developed using the QuEChERS method for residual organochlorine pesticides (OCPs) in soil and oriental melon, green pepper and lettuce. Recovery of OCPs in greenhouse soil and oriental melon, green pepper, and lettuce ranged from 73.3-110.6%. Limit of detection (LOD) of OCPs in soil and 3 crops were 0.01-0.08 and $0.11-0.17{\mu}g/kg$. The residues of OCPs in oriental melon, green pepper and lettuce greenhouse soil were analyzed by the developed method, and dieldrin, ${\beta}-endosulfan$ and endosulfan sulfate were detected at 1.4-72.5, 0.1-78.7 and $0.0-214.1{\mu}g/kg$, respectively. The detection frequency of 3 compounds in soils were 52 (29.7%), 34 (19.4%) and 57 (32.6%) among 175 samples, respectively. However, these compounds were not detected in all crop samples. The residue level in 3 crops were lower than 1/58.8 of maximum residue level of them. These results showed that the OCPs residue in oriental melon, green pepper, and lettuce greenhouse soil were not as high as crop safety threatening.