A method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for neonicotinoid pesticide analysis in agricultural products. Four compounds (imidacloprid, clothianidin, acetamiprid, thiacloprid) were extracted with acetonitrile from agricultural products and cleaned up by NH2 solid-phase extraction procedure, and eluted with 0.1% formic acid in methanol/dichloromethane (5/95, v/v). The limit of detection and quantification were 0.0001-0.0005 mg/kg and 0.001 mg/kg, respectively. The mean recoveries of neonicotinoid pesticide from agricultural products were in the range of 90.7-100.9% and 94.4-99.8%, as spiked at 0.2 mg/kg and 0.02 mg/kg, respectively. This validation satisfied the national criteria for pesticide analytical methods. In summary, The present method is fast, precise and sensitive enough for the Positive List System (PLS), and we conclude that the method is also suitable for neonicotinoid pesticide determination in a wide range of agricultural products.
This study was conducted to monitor the residual pesticides on red pepper powder produced in five regions, which are the major producers of red pepper in Korea, such as Ham-pyeong, An-dong, Yeong-yang, Yeong-gwang, and Cheongyang from 2015 to 2016. Residual pesticides were detected on all samples. Among the 286 pesticides tested, 58 pesticides were detected, with the most frequently detected being chlorfenapyr (93.7%). Twelve types of pesticides (chlorfenapyr, cypermethrin, chlorpyrifos, pyraclostrobin, cyhalothrin, tebuconazole, bifenthrin, deltamethrin, fenvalerate, lufenuron, azoxystrobin, and indoxacarb) were detected in all regions, and 14 types of pesticides were used only in certain regions. An analysis of the residual pesticides showed that none of the pesticides detected exceeded the MRL (Maximum Residue Limits). The Positive List System (PLS) requirements were applied to eight pesticides that had no set MRLs. 0.01 mg/kg (PLS requirements) was exceeded in 12 cases. A comparison of the estimated daily intake (EDI) of pesticides with the acceptable daily intake (ADI) to access their risk revealed %ADI values of 0.001-0.756. Carbofuran showed the highest (0.756%), but most pesticides were below 1%. The results show that residual pesticides in red pepper powder are at safe levels.
Kim, Hyun Bok;Lee, Young Bo;Lim, Jung Dae;Lee, So Ra;Koo, Bon Woo;Kweon, Hae Yong
Korean Journal of Medicinal Crop Science
/
v.28
no.6
/
pp.435-444
/
2020
Background: As the Positive List System (PLS) is implemented in broad application to agricultural products, attention to the correct use of pesticides is also needed in the production of mulberry leaves and fruit. In this regard, three types of pesticides against mulberry popcorn disease were applied 2 - 3 times both in the field and greenhouses to prepare safety standards. Residual pesticide analysis was conducted on mulberry fruits and leaves. Methods and results: Three pesticieds, thiophanate-methyl, thiophanate-methyl·triflumizole and fluopyram registered as PLS pesticides for mulberry popcorn disease, were sprayed in the Wanju and in Buan regions, after which residual pesticide analysis was conducted using high-performance liquid chromatography (HPLC). As three pesticieds were either undetected or below the permissible level in mulberry fruit, demonstrating that they were suitable for safe spraying. However, 5.6 mg/kg of thiophanate-methyl was detected in the greenhouse after three application, which was slightly above maximum residue limit (MRL). Furthermore the level of thiophanate-methyl·triflumizole was higher than 0.2 mg/kg ("Gwasang No. 2" variety, spraying twice) or similar to 0.09 mg/kg ("Daesim" variety, spraying thrice) the permissible level (0.1T mg/kg) as the thiophanate-methyl was detected in mulberry leaves in the greenhouse. Conclusions: The spraying frequency for controlling mulberry popcorn disease in greenhouses should be limited to two times or less, especially when mulberry leaves are treated with thiophanate-methyl·triflumizole careful consideration is required if the leaves are to be used as food materials.
We assessed the pesticide residues in the medicinal agricultural products distributed in Korea. Pesticide residues in 72 samples were analyzed using the QuECheRS method for 339 pesticides, using GC-MS/MS and LC-MS/MS. The pesticide residues were below the maximum residues limit (MRL) in 42 samples (58.3%); however, they exceeded the MRL in 5 samples (6.9%). These included 43 types of pesticides; 20 fungicides and 23 insecticides were detected 75 times and 58 times, respectively. Tebuconazole and carbendazim were the most detected fungicides, each 11 times. The levels of acetamiprid, cadusafos, chlorpyrifos, flubendiamide, fluopyram, and triazophos exceeded the MRL in Gogi berry, Omija, and Reishi mushroom. All of them were positive list system (PLS) items that lacked pesticide residue standards. Therefore, authorities should monitor the distributed medicinal agricultural products.
Kim, Kyung-Je;Koh, Young-Woo;Im, Seung-Bin;Jin, Seong-Woo;Ha, Neul-I;Jeong, Hee-Gyeong;Jeong, Sang-Wook;Yun, Kyeong-Won;Seo, Kyoung-Sun
Journal of Mushroom
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v.18
no.4
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pp.380-386
/
2020
The study was conducted for the safety evaluation of 320 pesticide residues in 768 Lentinula edodes fruit body samples and 143 L. edodes media samples, which are distributed nationwide in South Korea. The monitoring method was the second of the multi-residue methods in the Korean Food Code. GC-ECD, GC-NPD, and GC-MSD were used as evaluation equipment for analysis. Single-analysis of the target pesticides was performed for mepiquat chloride. Through the analysis of collected L. edodes samples, pesticide residues were detected in total seven cases, including four L. edodes fruit body samples and three L. edodes media samples. The detected pesticide residues were carbendazim, diflubenzuron, fluopyram, and dinotefuran. In this study, carbendazim was detected in three L. edodes fruit body samples and one L. edodes media sample. The detected amount of carbendazim was 0.056, 0.17, 0.043, and 0.09 mg/kg, respectively. The amount of carbendazim in the collected L. edodes samples was detected below the MRLs (maximum residue level). The detected amounts of fluopyram and dinotefuran were 0.068 mg/kg and 0.06 mg/kg, respectively. Two pesticide residues were detected in the medium in one case. Mepiquat chloride was not detected in this study. These results suggested that residual pesticides were detected in a small number of collected L. edodes. However, the PLS for unregistered pesticides MRL was 0.01 ppm; therefore, we have to conduct research on preparing safety standards for mushrooms, including L. edodes.
Kim, Yeong-Jin;Kim, Jong-Hwan;Kwon, Young-Sang;Song, Jong-Wook;Seo, Jong-Su
Korean Journal of Environmental Agriculture
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v.36
no.4
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pp.279-287
/
2017
BACKGROUND: Many farmers who cultivate the strawberries for export have used agricultural chemicals which MRL (Maximum Residue Limits) of main export target countries or simultaneous multi-residue analysis in Korea have not been established. Among them, the cyenopyrafen and cyflumetofen were selected and applied to this study to determine the PHI (pre-harvest interval) which is appropriate to the PLS (Positive List System) criterion (0.01 mg/kg) and to investigate the residual amounts in the samples. In addition, Fifty pesticides were monitored to check up whether it is suitable or not for main export target countries. METHODS AND RESULTS: Cyenopyrafen and cyflumetofen were spayed out to the strawberries. Samples for residual analyses were taken for maximum 60 days. After sampling, they were extracted by the QuEChERS method and analyzed using the LC-MS/MS. Cyenopyrafen and cyflumetofen were detected in a range of 0.0106~2.6517 mg/kg and of 0.0005~1.4480 mg/kg, respectively. From this results, they were found to be suitable for PLS concentration after 30 or 45 days after spray. In addition, they were detected in most samples that were selected at random. Their concentrations were higher than the PLS criterion in the maximum twenty samples. Twelve of pesticides unsuitable for main export target countries have been detected in the monitoring of simultaneous multi-residue analysis. The result indicates they are unsuitable for export since they excesses over PLS criterion. CONCLUSION: The monitoring result showed it is necessary to establish the pesticide standards of safe use suitable for the PLS criterion. In addition, it is considered continues management and inspection are needed to solve problems caused by unsuitable pesticides in export strawberries.
Kyusuk Han;Byung-Sup Kim;Sae Jin Hong;Young Hun Lee
Journal of Bio-Environment Control
/
v.32
no.2
/
pp.172-180
/
2023
This study was carried out to determine the sprouting period of early and mid-season varieties, which includes 'Atlantic', 'Chubaek', and 'Superior', during the summer storage period in a semi-underground warehouse without cooling system. And also it was investigated the effect of chlorpropham [Propan-2-yl N-(3-chlorophenyl)carbamate, CIPC] treatment on the sprouting inhibition for the varieties. This study was conducted to figure out a sprout inhibitory effect when CIPC was applied to 1kg of the potato tubers at concentrations of 10 mg and 20 mg which are lower than the treatment concentrations of ca 30 mg prescribed by the positive list system (PLS). The internal temperature of the warehouse used in this experiment was lowered by 5℃ or more than the outside temperature. The difference between the lowest and highest temperature during the experiment throughout the day was 5℃. It showed the effect of reducing to 1/2 of the difference in outdoor temperature. As for the sprouting of potatoes, the extremely early variety 'Chubaek' sprouts appeared at the 6th week of storage of control and it was the fastest sprouting potato among the control groups of the varieties. Sprouting began to appear in the Superior at the 6th week of storage, while the 'Atlantic' sprouted at the 8th week of storage. The appearance of sprouts was suppressed in all treatment groups of 'Atlantic' and 'Superior' varieties in CIPC treatments. Sprouts were observed in all treatment groups of 'Chubaek' after the 7th week, but the elongations of the sprouts in tubers were completely inhibited until the 8th week of storage. 'Atlantic' and 'Superior' seemed to have a sprouting inhibitory effect even with a low CIPC concentration of 10 mg·kg-1, with the exception of extremely early variety 'Chubaek' that breaks out of the dormancy quickly. Although weight loss occurred continuously during storage, it was minor loss of 0.7-1.6%. There was no consistent trend for changes of the loss in the varieties and CIPC treatments. Most common pathological disorder was the dry rot during the experiment, but only few were affected. The use of the tubers treated at 18℃ and 90% RH for 10 days and the rack of refrigeration system which lead to lack of convection seemed to have suppressed the spread of pathogens.
BACKGROUND: Unintentional residual pesticide in soil derived from preceding crops and the transfer to succeeding crops was considered a critical barrier for positive list system (PLS). Thus, an uncertain risk is predicted for ethoprophos applied at cultivation of preceding crop (Korean cabbage) to succeeding crop (spinach). METHODS AND RESULTS: Ethoprophos was treated on soil following the recommended dose and 5 times dose according to the safe use guidelines for Korean cabbage after seeding. On the 4 days after harvesting of preceding crop, spinach was sowed. The initial residual amounts of ethoprophos on soil (7.081-19.493 mg/kg) were decreased to 3.832-7.218 mg/kg until the harvest of Korean cabbage, and then finally decreased to 0.011-0.079 mg/kg after spinach cultivation. The uptake rates of ethoprophos from soil by Korean cabbage were 0.01-0.03% and distributed to root (0.150-0.903 mg/kg) and shoot (0.021-0.151 mg/kg), respectively. The residual amounts of uptake and translocation from preceding crop cultivated soil to spinach edible part were found to be below LOQ. CONCLUSION: The plant back internal (PBI) for ethoprophos is not recommended during sequential cultivation of leafy vegetables, since the residual amounts of ethoprophos in spinach were less than MRL (0.02 mg/kg).
BACKGROUND: Prior to implementing a positive list system (PLS), there is a need to establish acceptable daily intake (ADI) and maximum residue limit (MRL) for veterinary drugs that have been approved a few decades ago in South Korea. On top of that, chronic dietary exposure assessment of veterinary drug residues should be performed to determine whether the use of these veterinary drugs would cause health concerns or not. METHODS AND RESULTS: To establish the ADI, the relevant toxicological data were collected from evaluation reports issued by international organizations. A slightly modified global estimate of chronic dietary exposure (GECDE) model was employed in the exposure assessment owing to the limited residual data. Therefore, only the ADI of ephedrine was established due to insufficient data for the other veterinary drugs. Thus, instead of ADI, the threshold of toxicological concern (TTC) value was used for the other drugs. Lastly, the hazard index (HI) was calculated, except for etizazole hydrochloride, due to the potential of mutagenicity. CONCLUSION(S): The HI values of ephedrine, menichlopholan, and anacolin were found to be as high as 6.4%, suggesting that chronic dietary exposure to the residues from these uses was unlikely to be a public health concern. Further research for exposure assessment of veterinary drug residues should be performed using up-todate Korean national health and nutrition examination survey (KNHANES) food consumption data. In addition, all relevant available data sources should be utilized for identifying the potentials of toxicity.
This study was conducted to understand the overall status of the monitoring program for pesticide residues in foods of South Korea. Further propositions for its improvement were made, and from this study, the status on this program can be summarized as follows. In South Korea, the Ministry of Food and Drug Safety (MFDS) is responsible for overall control of pesticide residue monitoring. Depending on the time of monitoring (sampling at distribution or production step), the government agency responsible for monitoring is different: MFDS, Regional Offices of Food and Drug Safety and local governments are responsible for monitoring of foods at the distribution step, while the National Agricultural Products Quality Management Service (NAQS) and local governments are responsible for monitoring of foods in the production step (partially at sale and distribution steps). According to purpose of monitoring, domestic monitoring programs could be divided into two types: MFDS's "Residue Survey" and NAQS's "National Residue Survey" are conducted mainly for risk assessment purposes and various monitoring programs by the Regional Offices of Food and Drug Safety and local governments are conducted mainly for regulation purposes. For imported foods, monitoring should be conducted at both steps of customs clearance and distribution: the MFDS and the Regional Offices of Food and Drug Safety are responsible for the former, and for the latter, local governments are also responsible. However, it appeared that systematic and consistent monitoring programs are not being conducted for imported foods at the distribution step. Based on the information described above and more detailed information included in this paper, the following proposals for improving the monitoring program were forwarded: i) further clarification of monitoring program purpose, ii) strengthening of the monitoring program for imported foods, iii) providing the public with monitoring results by publication of an annual report and database. It is thought that exhaustive review on the pesticide residue monitoring program and efforts for its improvement are needed in order to assure both food safety and the success of the recently begun positive list system (PLS).
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