• Korean Journal of Food Science and Technology
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• v.39 no.2
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• pp.114-121
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• 2007

The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

• 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 Food Science and Technology
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• v.46 no.1
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• pp.7-12
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• 2014

A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

• Korean Journal of Environmental Agriculture
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• v.22 no.2
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• pp.130-136
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• 2003

An organophosphorus insecticide, chlorpyrifos and an arylnitrile fungicide, chlorothalonil commonly used far apple were subjected to a residual investigation under field conditions to ensure safety of terminal residues at harvest. After pesticides were applied at standard rate in apple tree fer 15 days for chlorpyrifos and 30 days far chlorothalonil, persistence of their residues in apple was investigated by several interval. At harvest, residual concentrations of chlorpyrifos and chlorothalonil in apple were 1.3 and 2.4mg/kg, respectively, and the residue levels were higher than MRL 1.0 mg/kg in Korea. As well fitted by the first-oder kinetics, biological half-lives of the pesticide residues in apple were 9.3 days for chlorpyrifos and 32.2 days for chlorothalonil. During the storage, half-lives of chlorpyrifos and chlorothalonil were 35.0 and 56.3days at room temperature, and 120.7 and 182.8 days at 412, respectively. Distribution of chlorpyrifos residue in flesh, fruit skin and stalk cavity of each apple corresponded to 0.1% 22.8% and 77.1%, respectively. In case of chlorothalonil, residue in flesh, fruit skin and stalk cavity was 4.4%, 10.4% and 85.2%, respectively.

• Korean Journal of Environmental Agriculture
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• v.40 no.4
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• pp.353-358
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• 2021

BACKGROUND: Prochloraz has been widely used as an imidazole fungicide on fruits and vegetables in Korea. Analytical approaches to evaluate prochloraz residues in herbal medicine are required for their safety management. In this study, we developed a GC-ECD method for quantitative determination of prochloraz in Platycodi Radix. The metabolite 2,4,6-trichlorophenol (2,4,6-T) was used as a target compound to evaluate total prochloraz residues as it is categorized to a representative residue definition of prochloraz. All residues containing 2,4,6-T were converted to 2,4,6-T and subjected to GC-ECD. METHODS AND RESULTS: In order to verify the applicability, the method was optimized for determining prochloraz and it metabolite 2,4,6-T in Platycodi Radix. Prochloraz and its metabolite 2,4,6-T residuals were extracted using acetone. The extract was diluted with and partitioned directly into dichloromethane to remove polar co-extractives in the aqueous phase. The extract was decomposed to 2,4,6-T, and then the partitioned ion-associate was finally purified by optimized aminopropyl solid-phase extraction (SPE). The limits of quantitation of the method (MLOQs) were 0.04 mg/kg and 0.02 mg/kg, respectively for prochloraz and 2,4,6-T, considering the maximum residue level (MRL) of prochloraz as 0.05 mg/kg in Platycodi Radix. Recovery tests were carried out at two levels of concentration (MLOQ, 10 MLOQ) and resulted in good recoveries (82.1-89.7%). Good reproducibilities were obtained (coefficient of variation < 2.8%), and the linearities of calibration curves were reasonable (r² > 0.9986) in the range of 0.005-0.5 ㎍/mL. CONCLUSION(S): The method developed in this study was successfully validated to meet the guidelines required for quantitative determination of pesticides in herbal medicine. Thus, the method could be useful to monitor prochloraz institutionally in herbal medicine.

• Applied Biological Chemistry
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• v.8
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• pp.87-93
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• 1967

1) For the micro-analysis of mercury in plant materials, the method of Furutani was shown to be the simplest and most efficient way and the recovery of the assay was about 98%. 2) When the rice grain was soaked in 1/1000 diluted solution of organo-mercury fungicide for 8 hours at the end of March, the amounts of mercury residues in the brown rice and unhulled rice were 8.8 to $9.5\;{\mu}g/g$ seeds and 10.1 to $10.7\;{\mu}g/g$ seeds, respectively. 3) By washing the treated rice seeds with running water for three days, tile residual mercury concentration was reduced to 1/4 to 1/5; thus the mercury residues were 1.86 to $1.92\;{\mu}g/g$ for brown rice and 1.96 to $2.93\;{\mu}g/g$ for unhulled rice. 4) The residual mercury was present more in the unhulled rice than in the brown rice, either before or after washing of the treated seeds. 5) Among the different rice varieties, no difference was observed in mercury residues by seed treatment and washing.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.227-234
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• 2019

An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

• Korean Journal of Environmental Agriculture
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• v.37 no.1
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• pp.57-65
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• 2018

BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

• Korean Journal of Food Science and Technology
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• v.45 no.4
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• pp.409-415
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• 2013

Post-harvest fungicide residue was measured in citrus fruits. Samples were collected from local markets in Seoul and analyzed using liquid chromatography coupled with mass spectrometry (LC-MS). LC-MS results were validated for the assay of pesticides by using linearity, accuracy, precision, and limits of detection and quantification. The linearity in the concentration ranged from 0.005 to 2.0 mg/kg ($R^2$ >0.999). Sample recoveries ranged from 80.2 to 98.3% with relative standard deviations below 4.0% for spiking levels from 0.01 to 1.0 mg/kg. The limits of detection ranged between 0.002 and 0.008 mg/kg, and the limits of quantification ranged between 0.006 and 0.027 mg/kg. The highest residue levels for carbendazim, thiabendazole, imazalil, and azoxystrobin in citrus fruits were 0.541, 0.958, 0.721, and 0.052 mg/kg, respectively. The pesticide residues found in citrus fruits were blow maximum residue limits (MRLs) and are not a serious public health problem.

• Korean Journal of Environmental Agriculture
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• v.18 no.3
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• pp.215-220
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• 1999

Behaviour of a fungicide $^{14}C-propiconazole$ was investigated in a rice plant grown-lysimeter soil. The lysimeter was composed of soil cores of silty clay. $Propiconazole(Tilt\;250^R\;EC)$ plus $^{14}C-labeled$ propiconazole was applied on the surface of lysimeter soil at a rate of 0.12kg/10a after rice transplanting. The application was done consecutively for two years. The behaviours of propiconazole in the lysimeter soil were investigated by measuring the amounts of $^{14}C-leachate$, $^{14}CO_2$, the residues distributed in each soil segment and taken up by rice plants. The relative amounts of $^{14}C$ leached from the lysimeter were the background level of the applied $^{14}C$ throughout expeiment. The amounts of $^{14}CO_2$ evolved from the lysimeter were 5.7 and 7.8% of the original $^{14}C$ in the 1st and 2nd treatment, respectively. The amounts of volatile substances soil were the background level throughout experiment, which indicated that propiconazole was stable chemically in the experimental condition. The $^{14}C-activities$ absorbed and translocated into rice plants were 3.7 and 7.6% in 1st and 2nd treatment, respectively. The $^{14}C-activities$ in the soil layer of the lysimeter was distributed mainly in the depth of 0 to 20cm, which suggested propiconazole did not have the risk of groundwater contamination.