• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.32-40
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• 2015

This study was implemented to evaluate food safety on residual pesticides in agricultural products of Korea and to use as a data base for the establishment of food policy. A total of 196 pesticide upon these products were analyzed using multi class pesticide multiresidue methods of Korean Food Code, and 232 samples of 15 agricultural products collected from 9 regions were supplied for this study. In the results, 64 kinds of pesticides were detected in 53 samples, chlorpyrifos and procymidone of them were shown a high frequency of detection in the analyzed pesticides. Among them, two samples (chlorpyrifos in perilla leaves and picoxystrobin in peach) were detected over Maximum Residue Limits (MRLs). The levels of the detected pesticide residues were within safe levels. Also, the intake assessment for pesticide residues including chlorpyrifos at multi pesticide residue monitoring were carried out. The result showed that the ratio of EDI (estimated daily intake) to ADI (acceptable daily intake) was 0.001~0.902% which means that the detected pesticide residues were in a safe range so that residual pesticides in the agricultural products in Korea are properly controlled.

• Journal of Food Hygiene and Safety
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• v.19 no.1
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• pp.12-18
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• 2004

Ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin in chicken muscle were seperated by liquid extraction and determined with high performance liquid chromatography (HPLC) with fluorescence detector. Analysis was carried out using following conditions; Cl8 column (250${\times}$4.6 mm i.d. 5 ${\mu}{\textrm}{m}$ particle size), mobile phase composed of D.W. (containing 0.4% triethylamine and phospholic acid): methanol : acetonitrile (800:100:100, v/v/v), isocratic pump at a flow rate of 1.0 $m\ell$/min and 50 ${mu}ell$ of injection volume, fluorescence detector with EX278 nm/EM.456 nm. The calibration curves of four fluoroquinolones showed linearity (${\gamma}$$^2$$\geq$0.999) at concenration range of 0.025-0.6 $\mu\textrm{g}$/ml. The recoveries in fortified chicken muscle represented more than 80% with low coefficient of variation (〈10%) for concentration range of four fluoroquinolones. The detection limits for ofloxacin, norfloxacin, ciprofloxacin, and enrofloxacin were 23.5, 3.4, 3.0 and 2.5 ng/g in chicken muscle, respectively. We also monitored fluoroquinolones residue in muscle of chickens (broiler 1:227, Korean native chicken 219, laying chicken 77) using EEC-4-plate screening and HPLC conformation methods. Ten(broiler 5, Korean native chicken 5) out of the fifteen samples which were positively detected by EEC-plate screening method from 1,523 chicken meat were confirmed with ciprofloxacin and enrofloxacin by HPLC. The ranges of residual concentration were 0-0.12 ppm for ciprofloxacin and 0.01-6.79 ppm for enrofloxacin. In conclusion, our method could be applied effectively to determine four fluoroquinolones residues in chicken meat, and further survey for fluoroquinolones residue in chicken meat are needed for more effective control of fluoroquinolones used in livestock.

• Journal of Food Hygiene and Safety
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• v.36 no.5
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• pp.392-399
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• 2021

This study was conducted to research the status of pesticide residues in a total of 114 herbs and spices obtained from January to October 2020. 341 pesticide residues were analyzed by the multi class pesticide multiresidue methods using GC-MSMS, GC-ECD, GC-NPD, LC-MSMS, LC-PDA, and LC-CAS. As a result of analysis, 36 pesticide residues were found, and detection rate was 31.6%. Of them, seven samples were detected over Maximum Residue Limits (MRLs) and the unsuitable level in pesticide was 6.1%. The herbs and spices exceeding MRLs include coriander (2 times), mint (2 times), basil (once), rosemary (once), and boraye (once). According to an analysis of 341 pesticide residues, 22 pesticides were detected 52 times and 8 pesticides were found to exceed the MRLs. The pesticides exceeding MRLs were ingredients such as etofenprox, flufenoxuron, fluquinconazole, iprodione, lufenuron, paclobutrazol, phenthoate, and spiromesifen.

• 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.

• 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.38 no.3
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• pp.112-122
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• 2023

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.

• Journal of Food Hygiene and Safety
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• v.38 no.6
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• pp.489-495
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• 2023

In this study, we detected the presence of residual pesticides in 341 agricultural products collected from local food outlets in western Gyeonggi Province. Residual pesticides were detected in 105 (30.8%) samples. Six samples exceeded the legal limits for residual pesticides, resulting in a non-compliance rate of 1.8%, which was slightly higher than the average non-compliance rate of 1.4% in the last three years. Among the tested agricultural products, only fruits and vegetables were found to have pesticide residues, with 24 of 34 fruits (a detection rate of 70.6%) and 81 of 277 vegetables (a detection rate of 29.2%) testing positive. In total, 59 types of pesticides, including acetamiprid, which was detected 208 times, were detected and had a detection range of 0.01-2.38 mg/kg. Among the 105 agricultural products containing pesticide residues, a single pesticide was detected in 62 samples (59%) and two or more pesticides were detected in 43 samples (41%). In particular, 14 pesticides were detected in the same sample of peaches; dinotefuran was detected 21 times. Upon examining the toxicity of the detected pesticides, Class III pesticides (moderate toxicity) were detected 44 times (21.2%) and Class IV pesticides (low toxicity) were detected 164 times (78.8%). Class I, II, and III pesticides with fish toxicity were detected 68 (32.7%), 14 (6.7%), and 126 times (60.6%), respectively. Upon examining the exposure to high-frequency pesticide components detected five or more times, the hazard index was found to be ≤2.8%. Accordingly, the hazard of residual pesticides based on dietary intake was deemed insignificant.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.390-401
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• 2023

Major components of lac coloring include laccaic acids A, B, C, and E. The Korean Food Additive Code regulates the use of lac coloring and prohibits its use in ten types of food products including natural food products. Since no commercial standards are available for laccaic acids A, B, C, and E, a standard for lac pigment itself was used to separate laccaic acids from the lac pigment molecule. A standard for each laccaic acid was then obtained by fractionation. To obtain pure lac pigment for use in food by High performance Liquid Chromatography Photo Diode Array (PDA), a C8 column yielded the best resolution among various tested columns and mobile phases. A qualitative analytical method using High Performance Liquid Chromatography (HPLC) Tandem Mass(LC-MS/MS) was developed. The conditions for fast and precise sample preparation begin with extraction using methanol and 0.3% ammonium phosphate, followed by concentration. The degree of precision observed for the analyses of ham, tomato juice and Red pepper paste was 0.3-13.1% (Relative Standard Deviation (RSD%)), degree of accuracy was 90.3-122.2% with r²=0.999 or above, and recovery rate was 91.6-114.9%. The limit of detection was 0.01-0.15 ㎍/mL, and the limits of quantitation ranged from 0.02 to 0.47 ㎍/mL. Lac pigment was not detected in 117 food products in the 10 food categories for which the use of lac pigment is banned. Multiple laccaic acids were detected in 105 food products in 6 food categories that are allowed to use lac color. Lac pigment concentrations range from 0.08 to 16.67 ㎍/mL.

• 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.23 no.3
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• pp.239-247
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• 2008

Objective of this study was to investigate residual the levels of heavy metals in rice grain and soils of "Top-Rice" and common rice cultivation areas from 2005 to 2007. Soil and rice grain samples were taken from 33 "Top-rice" areas and neighboring paddies, and analyzed for the elements using ICP-OES and ICP-TOF-MS after acid digestion. A concentration of arsenic in paddy soil was 1.33 mg/kg which was below 1/5-1/11 fold of the threshold levels(concern: 4 mg/kg, action: 10 mg/kg), and paddy soil was 0.06 mg/kg of Cd(cadmium) being below 1/25-1/67 fold of the limits(concern: 1.5 mg/kg, action: 4 mg/kg). A level of Cu(copper) in paddy soil was 4.57 mg/kg which was below 1/11-1/27 fold of the threshold levels(concern: 50 mg/kg, action: 125 mg/kg), and Pb(lead) concentration in paddy soil was found to be a 4.68 mg/kg. In addition, Hg(mercury) concentration in paddy soil was to be a 0.03 mg/kg, which was below 1/131-1/328 fold of the threshold levels(concern: 4 mg/kg, action: 10 mg/kg). The average concentrations of As, Cd, Cu, Pb and Hg in the polished rice samples were 0.037, 0.043, 0.280, 0.048 and 0.002 mg/kg, respectively. These levels are lower than those of other countries in rice grains. Assuming the rice consumption of 205.7 g/day by total dietary supplements in Korea, the amount of total weekly metal intake of As, Cd, Cu, Pb and Hg by polished rice were estimated to be 0.0892, 1.035, 6.712, 1.161 and 0.054 ${\mu}g/kg$ body weigh/week, respectively. The PTWI(%) of As, Cd, Cu, Pb and Hg were 5.95(inorganic arsenic), 0.26(total arsenic), 14.79, 0.19, 4.65 and 1.07% estimated to be 0.0892, 1.035, 6.712, 1.161 and 0.054 ${\mu}g/kg$ body weigh/week, respectively. In conclusion, it was appeared that the heavy metals contamination in the brown and polished rice should not be worried in Korea.