• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.30-39
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• 2019

An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.

• 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.2
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• pp.140-147
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• 2019

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.39 no.2
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• pp.118-127
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• 2024

This study investigated the levels of 345 pesticide residues in 50 herbal medicines sold in Incheon metropolitan city to determine their safety. Pesticide residues are harmful substances that can cause serious health problems owing to their toxicity and carcinogenicity. The analysis of pesticide residues in the samples was conducted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, known for its high analysis efficiency, to analyze a wide range of pesticides for which no standards have been set. The analysis was cross-validated with the pretreatment method outlined in the Korea Pharmacopoeia. Among the 50 samples encompassing 24 different herbs, 22 pesticide residues were detected in 24 samples, covering 7 distinct herbs, resulting in a detection rate of 48%. It is noteworthy that, except for two cases, all detected pesticides were those for which no standards were set. However, after conducting a risk evaluation considering the daily dosage of herb, it was determined that the levels of pesticide residues were within safe limits. Pesticides with high frequency within the same category of herbs were detected, indicating the necessity for continuous monitoring and regulation. In addition, comparative analysis using the pretreatment method outlined in the Korean Pharmacopoeia, yielded similar results, suggesting the possibility of analyzing pesticide residues in herbs using the QuEChERS method. The study emphasizes the importance of continuous monitoring of pesticide residues in herbs and the development of high-efficiency reliability analysis methods should continue to ensure consumer safety.

• Journal of Food Hygiene and Safety
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• v.29 no.3
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• pp.170-180
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• 2014

The aim of this study was to investigate pesticide residues in 2,877 market vegetables in the northern area of Seoul in 2013. Pesticide residues in the samples were analysed by multiresidue method for 285 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. 385 samples(13.4%) were detected with pesticide residues at or below MRL, and 15 samples(0.5%) were found to detect pesticide residues exceeding MRL. The most frequently detected samples were sedum(63.6%), chamnamul(45.8%), leek(44.5%) and green&red pepper(30.8%). Among the 15 violated samples, leek(5 cases) and welsh onion(4 cases) showed the highest violation rate. A total of 74 samples(18.5%) contained multiple pesticide residues in one vegetable. Procymidone, chlorofenapyr and cypermethrin were the pesticide most frequently found. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated into the range of 1.05~28.61%. The results have meant that there was no health risk through dieting commercial agricultural products detected with pesticide residues.

• The Korean Journal of Pesticide Science
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• v.14 no.2
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• pp.86-94
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• 2010

This study was conducted to monitor the current status of pesticide residues in agricultural products before auction at whole markets in Busan area from March 2006 to December 2008. Of the 7,237 samples that were analyzed by multiresidue methods, 1,164 samples (16.1%) had pesticide residues and 231 samples (3.2%) exceeded the maximum residue limits (MRLs). 181 samples of the 231 samples exceeding MRLs were applied to the tentative limits because the use of the pesticides for the agricultural products was not established against the MRLs in the Korea Food Code, and it is equivalent to 78.4%. The order of pesticides exceeding MRLs was endosulfan, procymidone, chlorothalonil, ethoprophos, chlorpyrifos, diethofencarb, kresoxim-methyl and EPN. Of 211 samples with two or more pesticides residues, the residues exceeded the MRLs in 80 samples and it is equivalent to 37.9%. This study results suggested that pesticide residues exceeding MRLs could be attributed to the use of inapplicable pesticides for agricultural products and the use of two or more pesticides.

• 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.

• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.21-27
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• 2012

Dietary exposure assessment by ages was performed in this study using pesticide residues data examined in vegetable commodities collected in Seoul from 2007 to 2009, and the vegetable intakes for Seoulites which were obtained after analysing the Korea National Health and Nutrition examination survey data of 2008. There was a statistical difference for vegetable intakes by ages (P<0.001). Vegetable intake was the highest in 40~59 age group and was the lowest in under 5 age group. The %ADI was calculated using vegetable pesticide residues and vegetable intake for Seoulites by ages. Considering below 1 of the %ADI by ages, the risk caused by pesticide residues in vegetables was very low and vegetable intake was safe.

• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.43-53
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• 2012

In order to monitor the levels of pesticides in environment-friendly stalk and stem vegetables and leafy vegetables selling at markets in Korea. A total of 637 (395 organic agricultural products, 242 pesticide-free agricultural products) samples of 21 stalk and stem vegetables and leafy vegetables were collected twice from markets in July and August 2010 in Korea. Pesticide residues in samples were analyzed by multiresidue method for 240 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. The suspected-pesticides were confirmed with a GC-MSD. As a result of analysis, six pesticides were detected from eight samples, representing a detection rate of 1.3% and amounts of pesticide residues in samples were as follows: alachlor 0.043, chlorfenapyr 0.022-0.324, diazinon 0.024, dicofol 0.009-0.138, dithiopyr 0.008, metolachlor 0.025 mg/kg. Their residue levels were below the MRLs. Estimated daily intakes (EDIs) of the pesticides detected from stalk and stem vegetables and leafy vegetables were less than 25% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe for consumption. However, five samples containing pesticide residues were unsuitable environment-friendly products because of pesticides detected more than their 10% MRLs in organic and pesticide-free agricultural products.