• Journal of Food Hygiene and Safety
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• v.35 no.2
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• pp.109-117
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• 2020

This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL-71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C₁₈ and primary secondary amine (PSA). Calibration linearity was obtained (r²>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

• Food Science and Preservation
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• v.21 no.1
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• pp.69-74
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• 2014

We tested for residual pesticide levels in school foodservice agricultural products in Seoul, Korea from 2010 to 2012. A total of 316 samples of 23 different types of agricultural products were analyzed via gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography-ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze 185 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 26 samples (8.2%), of which 6 samples (1.9%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in more than 65% of the Chwinamul, while 6 among 9 analyzed samples contained pesticide residue, and 1 sample exceeded the Korea MRLs. Among the 185 kinds of pesticides that we have tested, 18 were detected, while 7 of them were detected more than twice. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The most critical commodity is carbofuran in the perilla leaves, which has contributed 3.8% to the hazard index (HI). These results showed that the detected pesticides could not be considered as a serious public health problem. Nevertheless, constant supervision is recommended.

• The Korean Journal of Pesticide Science
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• v.11 no.3
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• pp.154-163
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• 2007

In order to elucidate the residual characteristics of some pyrethroid insecticides commonly used for Korean cabbage, such as bifentbrin, lambda-cyhalothrin and deltametbrin, the test pesticides were sprayed onto the crop at recommended rate and doubled rate of the recommendation. Their detection limits were 0.004 mg $kg^{-1}$ and mean recoveries at the fortification levels of 0.04 and 0.2 mg $kg^{-1}$ were from 95.16 to 99.32 and from 86.81 to 103.73%, respectively. Half-lives were from 2.5 to 3.6 at the recommended rate and from 2.3 to 3.9 days at the doubled rate of the recommendation. Initial residue amounts of bifenthrin and lambda-cyhalothrin at the recommended rate and doubled rate of recommendation and of deltamethrin at the recommended rate were less than their MRL, whereas, in case of deltamethrin sprayed at doubled rate of the recommendation, the residue level exceeded its MRL. However, the residue levels of the pesticides in the crop sampled at harvest were less than their maximum residue levels and the ratios of the estimated daily intake (EDI) to acceptable daily intake (ADI) for the pesticides tested calculated from the residue data at harvest were less than 7%, suggesting that these pesticides would be safe for Korean cabbage from the residue concern.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.335-349
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• 2011

100 residual pesticides in 1,565 medicinal herbs being on sale in Seoul was analyzed by a simultaneous multiresidue method. The recovery ratio was 71.0~119.7%. The detection rate of pesticide residues was 5.3% and the rate of excess to Maximum Residue Limits (MRLs) was 0.9% of the total samples. The medicinal herbs which had the high detection rate of residual pesticides were Alismatis Rhizoma, Citri Unshii Pericarpium, Lycii Fructus and Zyzyphi Fructus. The medicinal herbs detected pesticide over Maximum Residue Limits (MRLs) were Alismatis Rhizoma (4), Cnidii Rhizomain (4), Chrysanthemi Zawadski Herba (1), Citri Unshii Pericarpium (1), Lycii Radix Cortex (1), Menthae Herba (1), Schisandrae Fructus (1) and Taraxaci Herba (1). The residual pesticides which had the high detection frequency were cypermethrin, chlorpyrifos, phenthoate, endosulfan, isoprothiolane, chlorothalonil and chlorfenapyr. Estimated Daily Intake (EDI) of detected pesticides was compared to Acceptable Daily Intake (ADI) in order to assess risk. Ethoprophos detected in Cnidii Rhizomain showed the highest %ADI, 26.85. And pyraclofos and endosulfan in Cnidii Rhizomain, endosulfan and isoprothiolane in Alismatis Rhizoma and cyprodinil in Taraxaci Herba showed more than 1 %ADI, but others showed below 1 %ADI.

• Journal of Food Hygiene and Safety
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• v.37 no.2
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• pp.69-79
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• 2022

The purpose of this study is to monitor the pesticide residues in frozen fruits and vegetables distributed and sold in online and offline markets in Korea. For the study, 107 samples of 34 types of frozen fruits and vegetables were examined, and a total of 341 pesticide residues were analyzed by using multiclass pesticide multi-residue methods of the Korean Food Code. As a result, pesticide residues were detected from 16 of 64 frozen fruits samples and 15 of 43 frozen vegetables samples. Conclusively, residues were detected from 31 samples in total, showing a detection rate of 29.0%. Specifically, pyridaben exceeded the Maximum Residue Limits (MRLs) based on the Positive list system (PLS) in one of the frozen radish leaves, and the violation rate was 0.9%. Detection on frozen fruits and vegetables was made 23 times for 11 types and 36 times for 21 types. In total, 28 types of pesticide residues were detected 59 times. Fungicides were detected the most in frozen fruits, while insecticides were detected the most in frozen vegetables. The most detected pesticides were the insecticide, acaricide chlorfenapyr (5) and the fungicide boscalid (5). Chlorfenapyr was detected only in frozen vegetables, and boscalid was detected in frozen fruits except one.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.48 no.2
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• pp.158-167
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• 2015

A lateral flow immunoassay kit based on antigen-antibody interactions was developed to detect residues of beta-lactams, quinolones, tetracyclines, and sulfonamides in farmed fish. Group-specific antibodies showing cross-reactivity with other antibiotics in the same group were produced in rabbits. The rabbits were immunized eight times to obtain the maximum titers. Antibodies were extracted from the antisera collected from the immunized rabbits and produced group-specific reactions with antibiotics from the four groups. A kit was prepared that optimize conditions for the antigen-antibody reaction, using colloidal gold conjugated antibodies, and was designed to detect the four groups of antibiotics simultaneously. The kit enabled the detection of antibiotics in the four groups at below maximum residue limits (MRLs), which were $200{\mu}g/kg$ for tetracyclines, $100{\mu}g/kg$ for sulfonamides, $50{\mu}g/kg$ for beta-lactams, and $100{\mu}g/kg$ for quinolones. The cross-reactivity of the antibodies ranged from 10-80% for the sulfonamides, 20-100% for tetracyclines, 38-100% for quinolones, and 20-100% for the beta-lactams, confirming that the antibodies were group specific. The test kit was used 30 times to examine spiked antibiotics at the limits of detection (LODs) and all produced positive results, indicating high sensitivity. The LODs for the assay ranged from 4-20 ng/mL for beta-lactams, 25-50 ng/mL for sulfonamides, 20-100 ng/mL for tetracyclines, and 30-80 ng/mL for quinolones, and there were no false negative reactions at above these LODs. In addition, all of the LODs of the developed kit were correlated with high-performance liquid chromatography (HPLC) data. Our lateral flow immunoassay kit can simultaneously detect antibiotic residues from a large number of fish samples rapidly, strengthening the safety of domestic farmed and imported fish.

• Korean Journal of Environmental Agriculture
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• v.34 no.4
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• pp.303-308
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• 2015

BACKGROUND: Recently, various rice by milling degree is sold for health and taste. To provide safe food to consumers, it is need to know the change of heavy metal contents according to milling degree of rice.METHODS AND RESULTS: This study was to investigate residual the levels of cadmium (Cd), lead (Pb), copper (Cu) and zinc (Zn) as stated in the milling degree of the rice contaminated Cd and Pb from 2011 to 2012 in Chungcheongnam-do. Rice samples exceeded the maximum residue limits (MRL) of Cd and Pb were milled by five degrees (0.0, 2.45, 8.02, 10.48, 15.09%). Milled rice was digested by microwave method, and analyzed heavy metal contents using ICP-OES. Recovery ratios of 4 heavy metals such as Cd, Pb, Cu and Zn were ranged for 79.7-98.9%, and limits of detection (LOD) and limits of quantitation (LOQ) were fulfilled with the normal analytical standards. Concentrations of Cd, Pb, Cu and Zn were ranged 0.416-0.433 mg/kg, 0.183-0.26 mg/kg, 3.639- 3.882 mg/kg and 16.868-19.801 mg/kg, respectively.CONCLUSION: From these results, conforming with increase of milling degree of rice, Cd, Pb, Cu, and Zn contents tended to decrease. The contents of heavy metals were decreased 3.1% in Cd, 29.3% in Pb, 6.4% in Cu and 15.1% in Zn, in according to the highest milling degree of 15.09%.

• Korean Journal of Environmental Agriculture
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• v.36 no.4
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• pp.279-287
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• 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.

• Korean Journal of Food Science and Technology
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• v.42 no.1
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• pp.1-7
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• 2010

To revise the dithiocarbamates residue analysis method and survey the residues in agricultural products that were treated with these fungicides in Korea, we purchased 20 types of foodstuffs (rice, potato, cabbage, apple etc.) from markets in five major cities. 236 samples of the purchased foodstuffs were then analyzed for the presence of dithiocarbamates by HPLC/UV and HPLC/APCI-MS. The $R^2$, LOD and LOQ in the range of 0.5-107.3 mg/L were as follows: DCC: y=174.34x+18.315, $R^2=0.9999$, 0.01 mg/L, and 0.04 mg/L; EBDC: y=227.38x-14.715, $R^2=1.0000$, 0.01 mg/L and 0.02 mg/L; PBDC: y=38.46x-21.412, $R^2=0.9999$, 0.04 mg/L, and 0.1 mg/L; ETU: y=52.752x-4.4819, $R^2=0.9998$, 0.02 mg/L and 0.03 mg/L; PTU: y=128.28x+4.4624, $R^2=0.9998$, 0.02 mg/L, and 0.04 mg/L. The levels of DDC, EBDC, PBDC, ETU and PTU in 20 agricultural products fortified to 10.0-107.3 mg/L ranged from 61.7-117.5%, 65.3-110.1%, 61.5-109.6%, 69.3-116.3% and 70.2-97.2%, respectively. Overall, dithiocarbamates were detected in 100 samples and the detection ratio was 42.4%. Among these, only 3 samples (1.3%) of Lycii fructus had residue levels that were above the action limits, while the remaining samples (233 samples) contained levels of dithiocarbamates below the detection limit or below the Korea MRLs (Maximum Residue Limits).

• Food Science of Animal Resources
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• v.36 no.3
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• pp.319-325
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• 2016

This study was conducted to determine the residual amount of veterinary drugs such as meloxicam, flunixin, and tulathromycin in animal products (beef, pork, horsemeat, and milk). Veterinary drugs have been widely used in the rearing of livestock to prevent and treat diseases. A total of 152 samples were purchased from markets located in major Korean cities (Seoul, Busan, Incheon, Daegu, Daejeon, Gwangju, Ulsan and Jeju), including Jeju. Veterinary drugs were analyzed by liquid chromatography-tandem mass spectrometry according to the Korean Food Standards Code. The resulting data, which are located within 70-120% of recovery range and less than 20% of relative standard deviations, are in compliance with the criteria of CODEX. A total of five veterinary drugs were detected in 152 samples, giving a detection rate of approximately 3.3%; and no food source violated the guideline values. Our result indicated that most of the veterinary drug residues in animal products were below the maximum residue limits specified in Korea.