• The Korean Journal of Pesticide Science
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• v.13 no.2
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• pp.79-86
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• 2009

In order to elucidate the residual characteristics of the insecticides, bifenthrin and imidacloprid, the pesticides were sprayed onto the squash and their residues were analyzed with GC-ECD and HPLC. Detection limits of the pesticides were $0.005\;mg;kg^{-1}$ and recoveries of bifenthrin and imidacloprid in squash were from 100.87 to 104.31 and from 79.71 to 92.54%, respectively. Half-lives of bifenthrin and imidacloprid in squash were from 1.8 to 2.9 and from 1.5 to 2.5 days, respectively. Initial concentration of bifenthrin and imidacloprid sprayed at the recommended rate and double rate of recommendation were less than their MRLs. And also, residueal concentrations of the pesticides were rapidly decreased in squash with time. At harvest, estimated daily intakes (EDIs) of the pesticides were less than 0.6% of their acceptable daily intakes (ADIs).

• The Korean Journal of Pesticide Science
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• v.13 no.2
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• pp.98-104
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• 2009

This study was carried out to investigate the residue patterns of two neonicotinoid insecticides, dinotefuran and thiacloprid, commonly used for cucumber, were subjected to indicate a residual characteristic under greenhouse conditions. The pesticides were sprayed onto the crop at recommended and double doses 7 days before harvest and then sampling was done 0, 2, 3, 5, and 7 days after spraying. The amounts of their residues in the crop were analyzed with an HPLC. Their detection limits were 0.01 mg/kg for dinotefuran and 0.005 mg/kg for thiacloprid. Mean recoveries of dinotefuran and thiacloprid were from 85.78 to 89.52 and from 85.71 to 95.31%, respectively. Half-lives of dinotefuran and thiacloprid were 2.8 and 1.8 days at the recommended dose and 2.8 and 1.5 days at the doubled dose, respectively. The ratios of the EDI to ADI by intake the crop harvested 7 days after spraying were less than 0.1% of their ADIs.

• Journal of Food Hygiene and Safety
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• v.29 no.2
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• pp.131-140
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• 2014

The objective of this study was to develop a simultaneous method of 8 penicillin antibiotics including amoxicillin, ampicillin, cloxacillin, dicloxacillin, nafcillin, oxacillin, penicillin G and penicillin V in meat using LC-MS/MS. The procedure involves solid phase extraction with HLB cartridge and subsequent analysis by LC-MS/MS. To optimize MS analytical condition of 8 compounds, each parameter was established by multiple reaction monitoring in positive ion mode. The chromatographic separation was achieved on a $C_{18}$ column with a mobile phase of 0.05% formic acid and 0.05% formic acid in acetonitrile at a flow rate of 0.2 mL/min for 20 min with a gradient elution. The developed method was validated for specificity, linearity, accuracy and precision in beef, pork and chicken. The recoveries were 71.0~106%, and relative standard deviations (RSD) were 4.0~11.2%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.003~0.008 mg/kg and 0.01~0.03 mg/kg, respectively, that are below maximum residue limit (MRL) of the penicillins. This study also performed survey of residual penicillin antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Penicillins were not found in all the samples except a sample of pork which contained cloxacillin (concentration of 0.08 mg/kg) below the MRL (0.3 mg/kg).

• Journal of Food Hygiene and Safety
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• v.29 no.2
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• pp.123-130
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• 2014

A simultaneous determination was developed for 9 aminoglycoside antibiotics (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygromycin B, kanamycin, neomycin, spectinomycin, and streptomycin) in meat by liquid chromatography tandem mass spectrometry (LC-MS/MS). Each parameter was established by multiple reaction monitoring in positive ion mode. The developed method was validated for specificity, linearity, accuracy, and precision based on CODEX validation guideline. Linearity was over 0.98 with calibration curves of the mixed standards. Recovery of 9 aminoglycosides ranged on 60.5~114% for beef, 60.1~112% for pork and 63.8~131% for chicken. The limit of detection (LOD) and limit of quantification (LOQ) were 0.001~0.009 mg/kg and 0.006~0.03 mg/kg, respectively in livestock products including beef, pork and chicken. This study also performed survey of residual aminoglycoside antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Aminoglycosides were not found in any of the samples.

• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.246-253
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• 2011

This experiment was carried out to examine the residual amount variation of carbendazim and chlorpyrifos in fruit parts of red pepper according to the open field and/or the rain shelter house. It was shown higher residual amounts of agrochemicals in the field than the house condition at two hours (0 day) after chemical application, but it was shown higher residual amounts in the house at 5 days and 10 days. Although the residual amount in the field was higher than in the house at the beginning, the chemicals fast degraded in field condition. Carbendazim and chlorpyrifos remained as time passed in order of receptacle, but the residual amounts of two chemicals in leaf at $5^{th}$ day. Carbendazim and chlorpyrifos were lessened until 10 days after chemical application, and reduction rate were 19.1% and 66.4% in flesh, 45.2% and 62.3% in receptacle, and 41.6% and 72.0% in the stalk, respectively. The reduction rate at 15 days showed 31.1%, 75.3% in flesh, 43.5%, 81.7% in receptacle, and 47.7%, 82.8% in stalk, respectively. Therefore the reduction rate of carbendazim showed receptacle > stalk > flesh, and that of chlorpyrifos showed stalk > receptacle > flesh in order. The calculated half-life of carbendazim showed 29.6 days in flesh, 13.6 days in receptacle, and 16.0 days in stalk, but that of chlorpyrifos showed 8.3 days in flesh, 8.3 days in receptacle, and 6.3 days in stalk. In conclusion, the half-life of carbendazim was longer than that of chlorpyrifos in even part, and especially was longest in flesh part of fruit.

• The Korean Journal of Pesticide Science
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• v.20 no.3
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• pp.211-220
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• 2016

This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

• Journal of Food Hygiene and Safety
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• v.35 no.4
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• pp.365-374
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• 2020

This study was conducted to monitor the residual pesticides on a total of 320 stalk and stem vegetables from January 2019 to December 2019 in the Incheon metropolitan area. Pesticide residues in samples were analyzed by the multi-residue method for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Risk assessment was also carried out based on the amount of stalk and stem vegetables consumed. The linearity correlation coefficient for the calibration curve was 0.9951 to 1.0000, LOD 0.002 to 0.022 mg/kg, LOQ 0.005 to 0.066 mg/kg and recovery was 82.0 to 108.0%. According to the monitoring of pesticides, 36 (11.3%) of 320 were detected with pesticide residues and 3 (0.9%) samples exceeded the maximum residual limit. The detection frequency for Chinese chives and Welsh onion was higher than that for other stalk and stem vegetables. The frequently detected pesticides were etofenprox, procymidone, fludioxonil, and pendimethalin. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated in the range of 0.0062-24.1423%. These results indicate that there is no particular health risk through consumption of commercial stalk and stem vegetables detected with pesticide residues.

• 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).

• The Korean Journal of Pesticide Science
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• v.12 no.3
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• pp.229-235
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• 2008

Lack of honey bee toxicity data for most pesticide products used for strawberry restricts to predict the adverse effects to foraging honey bee after treatment of pesticide in plastic house. This study was conducted to evaluate the actual risk of worker honey bees (Apis mellifera L.) through acute contact toxicity test, acute oral toxicity test and toxicity of residues on foliage test with 21 pesticide products. The mortality of honeybee sprayed with 6 pesticides including dichlofluanid WP showed significantly different from control at recommended application rate in acute contact toxicity test at 24 hours after treatment. Fenpropathrin EC and milbemectin EC treatment groups showed more than 25% mortalities at recommended application rate in acute oral toxicity test. In toxicity of residues on foliage test, only fenpropathrin EC treatment group showed more than 25% mortalities at 10 days after treatment at recommended application rate. It was concluded that the most toxic route to exposure for honey bee is direct contact exposure to sprayed pesticides. Safety interval for honey bee was established by concerning the results of these tests.

• The Korean Journal of Pesticide Science
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• v.8 no.4
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• pp.280-287
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• 2004

We investigated the residual amounts of endosulfan and procymidone taken by vegetables grown in hydroponics culture and field conditions treated with the pesticides in order to evaluate safe cultivation concentration of the pesticides in the vegetables. Endosulfan and procymidone were selected as test pesticides because they have been reported to frequently detect in agricultural products at different concentrations. In hydroponic culture, by Chinese cabbage, procymidone was absorbed 3.8 times higher than endosulfan. The higher the pesticide concentration get, the worse the plant grew. In soil treated with 10 mg/kg of endosulfan, the pesticide absorbed by Leafy radish, Chinese cabbage and radish was less then their MRLs. In case of carlot, the residue level in soil which did not exceed its MRL was 1 mg/kg. The concentrations of procymidone in soil which did not exceed the MRLs in Leafy radish, Chinese cabbage, radish and carrot were 10, 10, 2 and 1 mg/kg, respectively Usually aged endosulfan and procymidone residues were less absorbed into crops than the fresh ones. Chinese cabbage absorbed more endosulfan and pocymidone than leafy radish, radish doing more than carrot.