• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.220-230
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• 2023

Imidacloprid is a neonicotinoid insecticide widely used for insect control in a variety of crops. The evaluation of imidacloprid total residues in animal feeds derived from crop by-products is required to ensure the safety of livestock products. We performed simultaneous LC/MS/MS analyses of imidacloprid and its metabolites in five different livestock products including beef, pork, chicken, milk and egg from domestic markets. The methods for sample preparation and instrumental analysis were established by modifying QuEChERS method to meet the Codex guidelines. The methods generated 0.0035 mg/kg of the limit of determination (LOD), 0.01 mg/kg of the limit of quantitation (LOQ) and standard calibration linearity with >0.983 of the coefficients of determination (R²). The methods exhibited the recovery values of imidacloprid and its metabolites ranging from 65.66 to 119.27% without any interference between matrices. Imidacloprid total residues in the livestock products were found as values lower than the LOQ and maximum residue limits (MRLs). This study suggests that the methods are successfully applicable for the safety evaluation of imidacloprid total residues in livestock products from domestic markets.

• Korean Journal of Food Science and Technology
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• v.53 no.4
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• pp.470-478
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• 2021

This study was conducted to monitor residual pesticides in a total of 527 school foodservice agricultural products from 2019 to 2020 in Incheon. Pesticide residues in the samples were analyzed by the multi-residue method in the Korean food code for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD, and HPLC-UVD. By monitoring the pesticides, 12 (2.3%) of the 527 pesticides were detected, and 2 (0.4%) samples exceeded the maximum residue limit. Twelve types of pesticides were detected in the agricultural products of carrot, chard, chili pepper, chwinamul, crown daisy, parsley, perilla leaves, and spinach. As a means of risk assessment through the consumption of agricultural products detected with pesticide residues, the proportion of estimated daily intake to acceptable daily intake was estimated in the range of 0.0000-39.7425%. Results showed no particular health risk through the consumption of school foodservice agricultural products with pesticide residues.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.283-289
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• 2019

This study was performed to monitor the residual pesticides in agricultural products used in school foodservice in the Gwangju metropolitan area. Risk assessment was also carried out based on the amount of agricultural products consumed. A total of 320 agricultural products supplied to schools in Gwangju were analyzed from 2015 to 2017. The pre-treatment and residual pesticide analysis of these products was conducted in accordance with the second method for multi-residue analysis of pesticides in the Korean food code. The hazard index was calculated by dividing the estimated daily intake (EDI) of pesticides by the acceptable daily intake (ADI). The linearity correlation coefficient for the calibration curve was 0.9923 to 1.0000, LOD 0.004 to 0.019 mg/kg, LOQ 0.012 to 0.057 mg/kg, and recovery was 79.1 to 100.2%. Residual pesticides were detected in 18 (5.6%) of 320 agricultural products used for school foodservice, and one sample of sweet potato stem (0.3%) exceeded the maximum residual limit (MRL). The detection frequency for chili peppers and bell peppers was higher than that for other agricultural products. The frequently-detected pesticides were boscalid and acetamiprid. These results showed that residual pesticide management is needed for chili pepper, bell pepper and sweet potato stem among agricultural products supplied to schools. The hazard index of bifenthrin in sweet potato stem showed the highest (64.18%), and the other pesticides were 0.03-8.23%. These results indicated that agricultural products supplied to schools in Gwangju were safe for consumption. To minimize the intake of residual pesticides, it is necessary to not only thoroughly wash agricultural products but to also ensure the expanded supply of products that are pesticide-free.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.30 no.2
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• pp.196-201
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• 2015

This study was conducted to monitor the current status of pesticide residues and to calculate the correlation between monthly price fluctuation and distribution of pesticide residues in leafy vegetables at the whole market in Gyeonggi-do from 2009 to 2013. From the result, the maximum residue limit (MRL) were frequently exceeded in 5 leafy vegetables which were 48 cases of crown daisy (5.8%), 28 cases of chard (5.1%), 28 cases of spinach (3.4%), 25 cases of perilla leaves (3.4%) and 24 cases of chamnamul (3.7%). The high rate of monthly pesticide residues exceeding MRL showed on crown daisy and chard observed in June and September, spinach in October to November and December to January, perilla leaves in July to August and January, and chamnamul in August to September. To calculate the correlation between monthly price fluctuation and distribution of pesticide residues, we performed the Pearson's correlation analysis. From the results, there were significant differences between monthly price and pesticide residues detected in chamnamul, spinach and perilla leaves (p < 0.05). There were also significant differences between monthly price and pesticide residues exceeding MRL in chamnamul and crown daisy (p < 0.05). Although the small number of leafy vegetables and short period were analyzed in this study, the consolidation monitor of pesticide residues according to the season and price will be needed to acquire the safety of agricultural products.

• The Korean Journal of Pesticide Science
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• v.12 no.4
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• pp.315-322
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• 2008

In this study, a simple, effective, and sensitive method has been developed for the quantitative residue analysis of cyhalofop-butyl and its metabolite cyhalofop acid in water and soil when kept under laboratory conditions. The content of cyholofop-butyl and cyhalofop acid in water and soil was analyzed by first purifying the compounds through liquid-liquid extraction and partitioning followed by Silica gel (adsorption) chromatography. Upon the completion of the purification step the residual levels were monitored through high-performance liquid chromatography (HPLC) using a UV absorbance detector. The recoveries of cyhalofop-butyl from three replicates spiked at two different concentrations ranged from 82.5 to 100.0% and from 66.7 to 97.9% in water and soil, respectively. The limit of detection and minimum detection level of cyhalofop-butyl in water and soil was 0.02 ppm and 10 ng, respectively. The recoveries of cyhalofop acid ranged from 80.7 to 104.8% in water and from 76.9 to 98.1 % in soil. The limit of detection of cyhalofop acid was 0.005 ppm in water and 0.01 ppm in soil, while the minimum detection level was 2 ng both in water and soil. The half-live of cyhalofop-butyl was 4.14 and 6.6 days in water and soil, respectively. The method was successfully applied to evaluate cyhalofop-butyl residues in water and soil applied aj. 30% emulsion, oil in water (EW) product.

• 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.34 no.2
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• pp.191-198
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• 2019

This study investigated the residual characteristics of bifenthrin and chlorothalonil in crown daisy and suggested pre-harvest residue limits (PHRLs) based on their dissipation patterns and biological half-lives. The samples for residue analysis were harvested at 0 (3 hr), 1, 3, 5, 7, 9, 11, 13, 15, 18, 22 and 26 days after treatment, and analyzed by $GC/{\mu}-ECD$ and TOF/MS. The limit of quantitation (LOQs) of bifenthrin and chlorothalonil were 0.0046 mg/kg and 0.0007 mg/kg, respectively. Recoveries ranged from $88.67{\pm}7.97%$ and $99.90{\pm}16.03%$, showing that this method is appropriate for the analysis of the pesticide residues in crown daisy. Being well within first order kinetics, the biological half-lives of the pesticide residues in crown daisy were 9.63 days for bifenthrin and 6.54 days for chlorothalonil. The PHRLs of bifenthrin and chlorothalonil were recommended as 11.70 mg/kg and 24.10 mg/kg for 26 days before harvest, respectively.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.

• The Korean Journal of Pesticide Science
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• v.14 no.1
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• pp.21-29
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• 2010

The analytical method for bifenazate was developed using a HPLC (UVD). Also, analytical condition of LC/MS was set up for bifenazate. We validated the method for the precision and the reproducibility. The correlation coefficient of bifenazate ranged from 0.05 to 2.5 mg/kg was 1.0. Limit of quantitation (LOQ) was 0.01 mg/kg. To measure recoveries from agricultural products such as foxtail millet (cereal grains), kidney bean (beans), orange (fruits), perilla leaves (vegetables) and oak mushroom (mushrooms), bifenazate was spiked. Mean recoveries of bifenazate for each sample were 82.7~104.1% at the level of 0.1 mg/kg and 73.1~104.3% at the level of 0.5 mg/kg. The relative standard deviations (n=3) were 0.2~9.7%. Pesticide residues for bifenazate were investigated in 16 commodities (rice, foxtail millet, buckwheat, kidney bean, peanut, sesame, orange, grapefruit, kiwifruit, spinach, perilla leaves, leek, garlic stem, garlic, ginger and oak mushroom) collected from 22 provinces in 2009. Bifenazate was analyzed using analytical method by HPLC from 304 samples, and residue was not detected.