• 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.

• Analytical Science and Technology
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• v.35 no.3
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• pp.136-142
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• 2022

According to media reports, the carcasses of euthanized abandoned dogs were processed at high temperature and pressure to make powder, and then used as feed materials (meat and bone meal), raising the possibility of residuals in the feed of the anesthetic ketamine and dexmedetomidine used for euthanasia. Therefore, a simultaneous analysis method using QuEChERS combined with high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry was developed for rapid residue analysis. The method developed in this study exhibited linearity of 0.999 and higher. Selectivity was evaluated by analyzing blank and spiked samples at the limit of quantification. The MRM chromatograms of blank samples were compared with those of spiked samples with the analyte, and there were no interferences at the respective retention times of ketamine and dexmedetomidine. The detection and quantitation limits of the instrument were 0.6 ㎍/L and 2 ㎍/L, respectively. The limit of quantitation for the method was 10 ㎍/kg. The results of the recovery test on meat and bone meal, meat meal, and pet food showed ketamine in the range of 80.48-98.63 % with less than 5.00 % RSD, and dexmedetomidine in the range of 72.75-93.00 % with less than 4.83 % RSD. As a result of collecting and analyzing six feeds, such as meat and bone meal, prepared at the time the raw material was distributed, 10.8 ㎍/kg of ketamine was detected in one sample of meat and bone meal, while dexmedetomidine was found to have a concentration below the limit of quantitation. It was confirmed that the detected sample was distributed before the safety issue was known, and thereafter, all the meat and bone meal made with the carcasses of euthanized abandoned dogs was recalled and completely discarded. To ensure the safety of the meat and bone meal, 32 samples of the meat and bone meal as well as compound feed were collected, and additional residue investigations were conducted for ketamine and dexmedetomidine. As a result of the analysis, no component was detected. However, through this investigation, it was confirmed that some animal drugs, such as anesthetics, can remain without decomposition even at high temperature and pressure; therefore, there is a need for further investigation of other potentially hazardous substances not controlled in the feed.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.149-158
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• 2022

This study aimed to investigate pesticide residues in 160 stalk and stem vegetables marketed in Northern Gyeonggi-do. The QuEChERS method using GC-MS/MS and LC-MS/MS was employed to analyze the residues of 341 pesticides in the samples. The maximum or lower than the residue limit was recorded in 75 samples (46.9%), while 4 samples (2.5%) exceeded the maximum residue limit (MRL). Thirty-nine kinds of residual pesticides were detected including fungicides (14), insecticides (22), herbicides (2), and plant growth regulator (1). Carbendazim and pendimethalin were the most frequelntly detected pesticides. Fenitrothion, procymidone, and diazinon exceeded MRL in garlic chives, and Welsh onion. This indicated that these vegetables along with water celery should be constantly monitored.

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.136-142
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• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.361-372
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• 2023

Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C₁₈) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

• Journal of Food Hygiene and Safety
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• v.39 no.3
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• pp.221-230
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• 2024

Pesticide residues were monitored in dried red pepper and pepper powder samples purchased in Northern Gyeonggi-do and from domestic online markets. The QuEChERS method was used to prepare 88 samples. GC-MS/MS and LC-MS/MS were used to analyze 338 pesticide residues. In the study, pesticide residues were detected in 70 samples (79.5%), with residues exceeding the maximum residue limits (MRL) in 4 samples (4.5%). Pesticide levels exceeded the MRL in imported samples, with two samples of dried red pepper and two samples of pepper powder showing elevated levels. Among the 61 pesticides detected, tebuconazole, a fungicide was most frequently detected (52 times). Tricyclazole, which is used to control the main disease affecting rice, exceeding the MRL in 3 of 12 Vietnam-origin samples. Ethion exceeded the MRL in one Indian-origin sample. Both tricyclazole and ethion are banned for use in pepper products in Korea and are regulated under the positive list system (PLS). Conversely, pesticides detected in domestic samples were within the MRLs. Therefore, authorities should monitor pesticide residues in imported red pepper products.

• Journal of Food Hygiene and Safety
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• v.39 no.3
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• pp.239-249
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• 2024

In this study, we investigated the concentrations of pesticide residues in agricultural products marketed in northern Seoul and assessed their potential health risks. A total of 1,737 samples were collected using the QuEChERS method, followed by LC-MS/MS and GC-MS/MS. Pesticide residues below the MRLs were detected in 560 samples of 72 items (32.2%), but 38 samples of 22 items had pesticide residues above the MRLs. Residual pesticides were detected in 53.8% of fruits, 33.0% of vegetables, 28.6% of herbs, 15.4% of beans, and 10.5% of rice samples. Most of the samples that exceeded the MRLs were vegetables, especially leafy, stalk, stem, and root vegetables; herbs and mushrooms also exceeded the permitted MRLs. Of the 105 pesticides investigated, dinotefuran, fluxametamide, chlorfenapyr, azoxystrobin, and carbendazim were the most frequently detected, whereas 23 pesticide residues, including terbufos, carbendazim, and fluxametamide, were detected above the MRL values. The hazard indices were calculated as 0.00003-1.31406%, which suggests that the investigated pesticide residues in the samples were within safe levels, but continuous monitoring of pesticides in agricultural products is needed to ensure the safety of consumers.

• Journal of Food Hygiene and Safety
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• v.37 no.6
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• pp.373-384
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• 2022

Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO₄ and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R²) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

• Korean Journal of Environmental Agriculture
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• v.36 no.3
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• pp.211-216
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• 2017

BACKGROUND:This study was conducted to investigate residual organochlorine pesticides (ROCPs) in agricultural soils and crops. Agricultural soil samples and crop samples were collected from 93 cities and counties. METHODS AND RESULTS: Extraction and clean-up for the quantitative analysis of ROCPs were conducted by the modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Recovery and limit of detection (LOD) of ROCPs in agriculturalsoils and crops were 76.5-103.0 and 75.2-93.2%, 0.01-0.08 and $0.10-0.15{\mu}g/kg$, respectively. Detected ROCPs in agricultural soils were ${\alpha}$-endosulfan, ${\beta}$-endosulfan, and endosulfan sulfate, the residue were 2.0-12.0, 1.2-53.1, and $2.2-329.8{\mu}g/kg$, respectively. But these pesticides in all green perilla leaf and green pepper samples were not detected. CONCLUSION: These results showed that ROCPs residues in agricultural soils were not as high as crop safety threatening.

• Animal Systematics, Evolution and Diversity
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• v.17 no.1
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• pp.49-57
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• 2001

The partial sequences of mtDNA cytochrome b gene in two subspecies of striped field mouse(Apodemus agrarius coreae and A. agrarius manchuricus) from Korea and northeast China were analyzed to determine the degree of genetic diversity in ech subspecies and to confirm their subspecific difference. In 18 specimens of A. agrarius coreae, ten haplotypes were resulted, and in two specimens of A. agrarius manchuricus. one haplotype was revealed. Tamura-Nei nucleotide distance among ten haplotypes in subspecies coreae ranged 0.36 to 1.86%. and nucleotide distance between two subspecies (coreae and manchuricus) was 0.37 to 1.47%: maximum infrasubspecific divergence in coreae was greater than maximum intersubspecific difference between two subspecies. Moreover, no major subgroup was resulted when 11 haplotypes in two subspecies were compared. Our sequence result was not cancordant with the morphological data studied so far, and it is concluded that cytochrome b gene sequence is not a good genetic marker to distinguish two subspecies of A. agrarius. In futurem, mtDNA control region analyses seemded to be necessary to reveal genetic relationship between these two subspecies of A. agrarius.