• The Korean Journal of Pesticide Science
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• v.15 no.3
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• pp.269-277
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• 2011

Recent outbreak of new diseases and pests which were introduced from abroad, seriously hampered both quality and safety of paprika fruits. This study has been carried out to aid an establishment of guideline for safe use of pesticides and reduction of their residues on paprika. Systemic fungicides boscalid and pyraclostrobin of either mixed (a.i.; 13.6+6.8%) or single (a.i.; 47 and 18.8%, respectively) water dispersible granule formulation(WG) products were sprayed with recommended or double dosage on paprika grown in green house at March and June. To draw pre-harvest residue limit, residues of each fungicide were analyzed from fruits collected eight times from 18 to 1 day pre-harvest. The biological half-lives of both boscalid and pyraclostrobin in mixed formulation in March and June were slightly shorter than those of single formulation which ranged from 14.4 to 20.1 days. Residue levels of both fungicides of single formulation in fruits in June were about one lower compared to those in March. However, application of double dosage frequently exceeded MRLs from fruits grown both seasons. These results showed that residue levels on fruits persisted longer period of time, more than two weeks, and so the case applied in winter season. The dissipation of fungicides on leaves and fruits was compared. The distribution of both fungicides in leaves was 20-200 times higher than that of fruits and persisted up to 18 days of pre-harvest period at the concentration of 10-40 ${\mu}g\;g^{-1}$. This study indicated that the mixed formulation product exhibited low residues in fruits, but high and long enough to pathogen growth in leaves.

• Analytical Science and Technology
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• v.27 no.3
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• pp.172-180
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• 2014

Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, and Monilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 and the maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues is required for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extracted with acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted with hexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LC-MS and quantified using external standard method. Linear range of fenpyrazamine was between $0.1{\sim}5.0{\mu}g/mL$ with the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked level of 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limit of detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that the developed and validated analytical method is possible for fenpyrazamine determination in agricultural product samples and will be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.31 no.3
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• pp.186-193
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• 2016

An analytical method was developed for the determination of oxathiapiprolin in agricultural commodities. Oxathiapiprolin is a new oomycide (fungicide of piperidinyl thiazole isoxazoline class) which controls downy mildew in cucurbits caused by Pseudoperonospora cubensis (oomycete plant pathogen). Agricultural commodities were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, adjusting pH between 9 and 10 by 1 N sodium hydroxide. After purification by silica SPE cartridge to clean up the interference of organic compounds, they were finally quantified by HPLC-UVD (high performance liquid chromatograph ultraviolet detector) using a wavelength at 260 nm and confirmed by LC-MS (liquid chromatograph mass spectrometer) in electro-spray ionization positive ion mode. The standard calibration curve was linear with coefficients of determination ($r^2$) 1.00 over the calibration ranges (0.025-2.5 mg/L). Recoveries were ranged between 86.7 to 112.7%, with relative standard deviations less than 10% at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates. The overall results were determined and estimated according to the CODEX guidelines (CAC/GL40). The proposed method for determination of oxathiapiprolin residues in agricultural commodities can be used as an official method.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.298-305
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• 2017

Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

• The Korean Journal of Pesticide Science
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• v.10 no.1
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• pp.15-21
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• 2006

In order to monitor the pesticide residues in/on peppers and pepper powder and to assess their risk, pesticides in/on green pepper from 10 farmgates and fresh red pepper from 9 farmgates in Chungbuk area and pepper powder from 6 wholesale markets in Cheongju city were analyzed with a GLC and an HPLC. Also, pepper powder made by pulverization of the dried red pepper was analyzed to elucidate the change of pesticide residues in fresh red pepper by oven-drying. The number of pesticides detected from peen pepper, fresh red pepper, dried red pepper and pepper powder were 9, 12, 12, and 17, respectively, including 10 pesticides (one fungicide and nine insecticides) which were exceeded the maximum residue limits (MRLs). The exceeding rate of the MRL were higher in dried red pepper and pepper powder than in green pepper and fresh red pepper. Although some pesticides in peppers and pepper powder exceeded the MRLs, their estimated daily intake(EDI) were less than 1.6% of their acceptable daily intakes(ADIs), suggesting that it would be estimated to safe. By oven-drying of fresh red pepper at $65^{\circ}C$ for 72 hours, the weight of dried red pepper was from 1/5.9 from 1/7.8 of fresh red pepper, while the concentration of pesticide residue in dried red pepper increased from 1.7 to 8.2 times, suggesting that further reconsideration was required for the MRL of pepper powder.

• The Korean Journal of Pesticide Science
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• v.21 no.1
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• pp.49-61
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• 2017

The study was conducted for safety evaluation of 208 kinds of residue pesticides on 200 dried agricultural products, which are distributed in Gwangju. The method of monitoring was the second of Multi Class Pesticide Multi-residue Methods in Korean Food Code, and GC-ECD, GC-NPD, GC-MSD, and LC-MS/MS were used as evaluation equipment to analyze. The residue level in pesticides were 15.5% (31 of 200 samples) and 4 samples exceeded MRLs. 4.5 mg/kg of pyraclostrobin (MRL; 3.0 mg/kg) was detected in red pepper, 1.49 mg/kg of chlorpyrifos (MRL; 0.13 mg/kg) in daikon leaves, 38.26 mg/kg of pyridalyl (MRL; 0.25 mg/kg) in pepper leaves, 0.98 mg/kg of chlorpyrifos (MRL; 0.05 mg/kg), respectively. Pesticides were found on the 15 samples among the 21 samples of red pepper which is a fruit vegetable, and this resulted in high detection rate of 71%. In addition, pesticides were detected on chwinamul, shitake, siler divaricata, daikon leaves and others within MRLs. The frequent detected kinds of pesticides were insecticide (47.6%), fungicide (33.3%), acaricide (14.3%), nematicide (4.8%) in the order named, and pesticides were methoxyfenozide > pyraclostrobin > azoxystrobin, chlorantraniprole > novaluron, trifloxystrobin in frequent order.

• 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 Environmental Agriculture
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• v.28 no.2
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• pp.194-201
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• 2009

To evaluate the exposure of non-point source pesticide pollution in agricultural watershed and to investigate pesticide distribution and runoff from agricultural land, paddy field, upland and orchard, this experiment was carry out during crop growing seasons. The pesticide were detected twenty pesticides fungicide 4, insecticide 10, herbicide 6) in water of Neungchon agricultural watershed and detection concentrations were range 0.008${\sim}$7.59 ppb. Most of the detection pesticides were using pesticides to rice paddy fields to control fungi, insects, weeds. During the crop cultivation, the pesticide were detected total thirty pesticides by pepper field soil 6, orchard soil 4, sesame field soil 3 and rice paddy field soil 5, and pesticide concentrations were range 0.001${\sim}$0.109 ppm. Especially the herbicides were detected mainly in May and June in the stream water. The pesticide were detected thirty pesticides by fungicide 2, insecticide 6, herbicide 5 in water of Jungam Koseong agricultural watershed and detection concentrations were range 0.01${\sim}$7.21 ppb. In regard to the detected pesticides, the concentration of individual pesticides measured in surface water of the study areas never exceeded guidelines for agriculture chemicals concerning water quality-effluent from paddy fields in Japan (Katayama, 2003). Runoff rate of pesticides was range 0.07${\sim}$3.06 % from Kongju agricultural land to watershed after applied pesticides.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.13-21
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• 2019

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination $(R^2){\geq}0.9906$, for streptomycin and dihydrostreptomycin. The mean recoveries at three fortification levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.235-241
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• 2019

An analytical method was developed for the determination of an antibiotic fungicide, kasugamycin, in agricultural products (hulled rice, potato, soybean, mandarin and green pepper) using liquid chromatographytandem mass spectrometry (LC-MS/MS). Samples were extracted with methanol adjusted to pH 13 using 1 N sodium hydroxide, and purified with a HLB (hydrophilic lipophilic balance) cartridge. Linearity of a matrix-matched calibration curve using seven concentration levels, from 0.001 to 0.1 mg/kg, was excellent with a correlation coefficient ($R^2$) of more than 0.9998. The limits of detection (LOD) and quantification (LOQ) of instrument were 0.0005 and $0.001{\mu}g/mL$, respectively, and the LOQ of analytical method calculated as 0.01 mg/kg. The average recoveries at three spiking levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) were in the range of 71.2~95.4% with relative standard deviation of less than 12.1%. The developed method was simple and all optimized results was satisfied with the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. The present study could be served as a reference for the establishment of maximum residue limits (MRL) of kasugamycin and be used as basic data for safety management relative to kasugamycin residues in imported and domestic agricultural products.