• Journal of Mushroom
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• v.18 no.4
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• pp.380-386
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• 2020

The study was conducted for the safety evaluation of 320 pesticide residues in 768 Lentinula edodes fruit body samples and 143 L. edodes media samples, which are distributed nationwide in South Korea. The monitoring method was the second of the multi-residue methods in the Korean Food Code. GC-ECD, GC-NPD, and GC-MSD were used as evaluation equipment for analysis. Single-analysis of the target pesticides was performed for mepiquat chloride. Through the analysis of collected L. edodes samples, pesticide residues were detected in total seven cases, including four L. edodes fruit body samples and three L. edodes media samples. The detected pesticide residues were carbendazim, diflubenzuron, fluopyram, and dinotefuran. In this study, carbendazim was detected in three L. edodes fruit body samples and one L. edodes media sample. The detected amount of carbendazim was 0.056, 0.17, 0.043, and 0.09 mg/kg, respectively. The amount of carbendazim in the collected L. edodes samples was detected below the MRLs (maximum residue level). The detected amounts of fluopyram and dinotefuran were 0.068 mg/kg and 0.06 mg/kg, respectively. Two pesticide residues were detected in the medium in one case. Mepiquat chloride was not detected in this study. These results suggested that residual pesticides were detected in a small number of collected L. edodes. However, the PLS for unregistered pesticides MRL was 0.01 ppm; therefore, we have to conduct research on preparing safety standards for mushrooms, including L. edodes.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.417-433
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• 2011

The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.

• The Korean Journal of Pesticide Science
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• v.9 no.4
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• pp.292-302
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• 2005

Condition of Ion-Trap gas chromatography-mass spectrometry (GC-MS) for rapid screening of 206-pesticides residues in agricultural foodstuffs was optimized. As applying a wide-bore column (10 m${\times}$0.53 mm, DF 0.25 um) connected with a fused silica restrictor (0.6 m${\times}$0.1 mm), a significant retention time reduction was obtained. Additionally, the shape of peaks was sharper and higher than classical GC's and GC-MS's, which allowed lower detection limits. To easily manage many spectral data, both of Electron Ionization(EI) and Chemical Ionization(CI) techniques were adopted in screening procedure. At the following steps, MS-MS technique were used to confirm screened analytes in complicated matrices.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.401-416
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• 2011

The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

• Journal of Environmental Science International
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• v.15 no.8
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• pp.811-817
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• 2006

We were carried out to monitor pesticide residues in herbal medicine. In Korea Pharmacy, these are no critics for pesticides except 5 kinds of organic chlorines (BHC, DDT, Aldrin, Endrin, Dieldrin) and heavy metals. We analysed 53 kinds of pesticides consisted of 14 kinds of organochlorines, 20 kinds of organophosphoruses, and 19 kinds of pesticides estimated endocrine disruptor on 373 samples consisted with 30kinds of herbal medicine. In this study, Domestic, Chinese and Japanese herbal medicines were tested with GC/ECD, GC/NPD and then confirmed with GC/MSD. Recoveries were 75$\sim$l10% in ECD detector and 76$\sim$97% in NPD detector. Detection limits were 0.004$\sim$0.064ppm in ECD detector and 0.006$\sim$0.094ppm in NPD detector. Organochlorines and others were not detected in samples.

• Journal of Applied Biological Chemistry
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• v.65 no.4
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• pp.413-419
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• 2022

The applicability of Brussels sprouts, which are widely cultivated in Jeju, as a functional biomaterial in the cosmetics and food industries is investigated. The active ingredients (total phenols and flavonoids, β-carotene, vitamin C, free sugar, minerals, glucosinolates, and isothiocyanates) and antioxidant activities of 70% ethanol extracts of Brussels sprouts and cabbage were analyzed. The total phenol, flavonoid, vitamin C, and β-carotene contents of Brussels sprouts were approximately 36%, 2.5 times, 2.3 times, and 65% higher than those of cabbage, respectively. The total free sugar content of Brussels sprouts was 58%-72% lower than that of cabbage. The K content was the highest among the other minerals, and there was little difference between the two samples. The Na content was approximately three times higher in cabbage than in Brussels sprouts. The total glucosinolate content of Brussels sprouts was 34.5 mol SE/g DW, twice that of cabbage. The sinigrin content of Brussels sprouts was thrice (10.06 μmol/g DW) that of cabbage. The isothiocyanate (sulforaphane, I3C) content in Brussels sprouts was double that of cabbage. The antioxidant activity of Brussels sprout extract was 2.5 to 2.8 times higher in 1,1-Diphenyl-2-picrylhydrazyl radical scavenging capacity and 3.3 to 3.6 times higher in 2,2'-Azino-bis(3-ethybenzothiazoline-6-sulfonic acid) radical scavenging capacity than those of cabbage extract. These are important basic data for the study of glucosinolates and isothiocyanates, which have anticancer activity, as well as antioxidant-related substances of Brussels sprout, which has high potential for use as a biomaterial in functional foods and cosmetics.

• The Korean Journal of Pesticide Science
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• v.20 no.1
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• pp.14-22
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• 2016

A trial of combining and quantifying the effects of food processing on various pesticides was carried out using a meta-analysis. In this study, weighted mean response ratios and confidence intervals about the reduction of pesticide residue levels in fruits and vegetables treated with various food processing techniques were calculated using a statistical tool of meta-analysis. The weighted mean response ratios for tap water washing, peeling, blanching (boiling) and oven drying were 0.52, 0.14, 0.34 and 0.46, respectively. Among the food processing methods, peeling showed the greatest effect on the reduction of pesticide residues. Pearsons's correlation coefficient (r=0.624) between weighted mean response ratios and octanolwater partition coefficients ($logP_{ow}$) for twelve pesticides processed with tap water washing was confirmed as having a positive correlation in the range of significance level of 0.05 (p=0.03). This means that a pesticide having the higher value of $logP_{ow}$ was observed as showing a higher weighted mean response ratio. These results could be used effectively as a reference data for processing factor in risk assessment and as an information for consumers on how to reduce pesticide residues in agricultural products.

• Journal of Food Hygiene and Safety
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• v.37 no.6
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• pp.373-384
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• 2022

Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO₄ and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R²) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

• The Korean Journal of Pesticide Science
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• v.19 no.3
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• pp.210-217
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• 2015

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.38 no.3
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• pp.131-139
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• 2023

In this study, we investigated pesticide residue levels in 535 domestically distributed agricultural products in South Korea using multi-residue analysis. Agricultural products from 13 regions, including Seoul, were pretreated using QuEChERS and d-SPE, and subsequently analyzed using LC-MS/MS and GC-MS/MS. Residual pesticides were detected in 288 (53.8%) out of the 535 samples, including 40 of apples, 40 of peppers, 33 of mandarins, 31 of peaches, and 144 other commodities. Furthermore, one sample of Korean cabbage exceeded the permitted maximum residue limit (MRL), diniconazole (0.18 mg/kg), detected at about twice the MRL. In total, 91 types of residual pesticides were detected, including fungicides (42), insecticides (48), and a nematicide. The most frequently detected pesticides were dinotefuran (91), carbendazim (75), tebuconazole (61), and pyraclostrobin (59). Our results showed that continuous monitoring of agricultural products is necessary.