• Journal of Dairy Science and Biotechnology
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• v.33 no.1
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• pp.27-34
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• 2015

The aim of this study was to optimize a simple, fast, and economic analytical method for the simultaneous determination of various pesticides (aldrin, p,p'-DDT, o,p'-DDT, p,p'-DDE, ${\alpha}$-endosulfan, ${\beta}$-endosulfan, dieldrin, heptachlor, permethrin, chlordane, deltamethrin, diazinon, bifenthrin, methoprene, propargite, fenpropathrin, cypermethrin, fenvalerate, and fenpropathrin) in milk by using dispersive solid phase extraction (SPE). In this study, two different extraction methods (low temperature cleanup and liquid-liquid partitioning), which were followed by a cleanup process based on dispersive-SPE, were evaluated and compared for the 19 pesticides. The results for all the pesticides were determined by gas chromatography mass spectrometry (GC/MS) with selected-ion monitoring mode, and the matrix effect of the method was evaluated. Comparison of these approaches yielded higher and more consistent recoveries of most pesticides at fortification levels of $1{\mu}g/mL$ using low-temperature fat precipitation, followed by cleanup process based on dispersive-SPE with PSA and C18 as sorbents, than other preparation process. The relative standard deviation was <20 % and the combination of this method were very effective for the cleanup.

• Korean Journal of Food Science and Technology
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• v.45 no.4
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• pp.391-402
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• 2013

Pesticide residues in agricultural products in Korea were evaluated to create a data base to inform food policy. Pesticide residues were investigated in 17 commodities collected from 9 provinces in 2012. Our analytical method of multiresidue analysis, involved the analysis of individual recovery, linearity, limit of detection, and limit of quantitation of 60 pesticides in six matrices. The pesticides, including acetamiprid and forchlorofenuron, were evaluated in 358 agricultural samples by liquid chromatography/tandem mass spectrometry. Twenty three pesticides were detected from 67 samples. The results showed that the ratio of estimated daily intake to acceptable daily intake was 0.00009-0.0861% by the intake assessment, which means that residual pesticides in agricultural products in Korea are properly controlled.

• The Korean Journal of Pesticide Science
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• v.13 no.4
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• pp.216-222
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• 2009

The present study aims to monitor pesticide residues in cut flowers collected from the farms and markets. Cut flowers used in this study included rose, lily and chrysanthemum collected from June to September, 2008. Samples were collected once from farms in Hwasung, Goyang (Gyeonggi-do), Inje (Gangwon-do) and thrice from wholesale market in Namdaemunm, Yangjae and Gangnam (Seoul). Total of 24 pesticides (12 fungicides, 11 pesticides and 1 acaricide) were detected from samples collected from farm and total of 64 pesticides (25 fungicides, 36 pesticides, 1 acaricide and 2 fungicides) were detected from samples collected from wholesale market. The highest detection frequency of pesticide from farm was for carbaryl (15%) and for boscalid, fluacrypyrin, fluquinconazole, methomyl, pyraclostrobin, trifloxystrohin (10%), with overall detection of $0.1-36.99\;mg\;kg^{-1}$. While the highest detection frequency of pesticides from wholesale market was for carbaryl, fluquinoconazole and kresoxim-methyl (18.52%), methomyl (16.6%), and methiocarb and thiacloprid (12.96%) with overall detection amount of $0.1-56.2\;mg\;kg^{-1}$. Higher amount of pesticides were detected in leaves than in flowers. Among the pesticides detected, detection frequency of unregistered pesticides for rose, chrysanthemum and lily was 55%, 60% and 63% collected from farms and 47%, 60% and 89% collected from markets, respectively. These pesticides require registration and further monitoring in floricultural crops.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.242-256
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• 2012

QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method has been a lot of research for pesticide analysis, because it is very simple and fast. However, this method requires high sensitivity instrument such as LC-MS/MS because of the use of small sample volume and many impurities compared to the conventional method. So, QuEChERS method needs to be modified for using with HPLC and GC-ECD/NPD. The aim of this work was to study the application of the QuEChERS method as well as its modification for the extraction and preconcentration of 5 groups of 61 pesticides from 4 fruits prior to their determination by HPLC-PDA, GC-ECD/NPD, and LC-MS/MS. The method was validated using spiking levels at 0.1 mg/kg (or 0.01 mg/kg) in apple, grapes, pear and persimmon. The average recovery by QuEChERS AOAC Official 2007. 01 version using the LC-MS/MS varied from 71.1127.4% for 61 pesticides. The average recovery rates using modified QuEChERS varied from 70.9~126% for 61 pesticides by HPLC-PDA and GC-ECD/NPD. The results satisfied the criteria of multiple pesticide residue analysis, setting 70~130% for recovery rates and below 30% for CV.

• Korean Journal of Environmental Agriculture
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• v.32 no.2
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• pp.142-147
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• 2013

BACKGROUND: This study was conducted to monitor residual pesticides in domestic agricultural products and to assess their risk to human health. METHODS AND RESULTS: 123 samples containing both general and environment-friendly certified agricultural products were purchased from traditional domestic markets and supermarkets in six provinces of Korea. Multiresidue analyses of one hundred twenty-two pesticides except for herbicides were performed with gas chromatography-electron capture detector, gas chromatography-nitrogen/phosphorus detector, and high-performance liquid chromatography. Sixteen pesticides were detected in 45 agricultural product samples, which were 38 general, 6 low pesticide and 1 of GAP agricultural product samples and the detection rate was 33.6%. Pesticides detected in agricultural product samples were cypermethrin, lufenuron, fenvalerate, bifenthrin, chlorfenapyr and iprodione. Residual concentration of 18 samples were exceeded the recommended maximum residue limit set by Ministry of Food and Drug Safety and two kinds of unregistered pesticides in korea were also detected in two samples. CONCLUSION(S): In order to do risk assessment by agricultural products consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to %ADI values. The range of %ADI values was from 0.038% to 2.748%. Taken together, it demonstrates the pesticides found in agricultural products samples were below the safety margin, indicating no effect on human health.

• The Korean Journal of Pesticide Science
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• v.17 no.4
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• pp.271-282
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• 2013

This is the result of pesticide residue monitoring certified Good Agricultural Practice (GAP) by national agricultural cooperative federation (NACF) from 2009 to 2012. NACF evaluated simultaneously 283 pesticide multi-analysis method with GC (ECD, NPD) and HPLC. 6,590 agricultural products were analyzed in this period. As the results 1) detected 20.27% in 2009, 23.42% in 2010, 28.07% in 2011 and finally 31.75% in 2012, respectively. There was the total detected pesticide residue in the agricultural products. The violated ratio of agricultural products were 2.25% in 2009, 1.82% in 2010, 1.67% in 2011 and 3.47% in 2012, respectively. 13 pesticides went over the maximum residue limits (MRLs); carbendazim was the predominant violation. 40 pesticides; endosulfan was the predominant detected pesticide did not registered respectively crops in Korea. Most agricultural products that were under the MRLs met the safety standard, however agricultural products that contain neither registered nor set up MRL any level for example endosulfan in strawberry. Agricultural products that go over the MRLs with permitted pesticides, for example carbendazim in apple, are rejected. Because of these intricacies continual observation and evaluation will be need during GAP agricultural cultivation.

• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.28-34
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• 2012

We analysed 149 samples of Korean traditional herbal tea materials. The 156 pesticides were analyzed by GC/ECD and NPD, detected pesticides were confirmed by GC-TOF/MS. Sample preparation was performed bv multi-residue analysis method of multiclass pesticides of the Korea Food Code. The residual pesticides were detected in 22 samples(14.8%), the highest detection frequency samples are lycium and jujube. Detected pesticides in Korean traditional herbal tea materials were chlorpyrifos (5 samples), chlorothalonil (3 samples), cypermethrin (3 samples), hexaconazol (3 samples) and cyhalothrin(3 samples). The pesticide types detected in Korean traditional herbal tea materials were organophosphorus(29.2%), pyrethroids(16.7%), organochlorines (12.5%) and triazoles(12.5%). The 5 samples(lycium, jujube, chrysanthemum, balloon-flower, milk vetch root) were detected pesticides below MRLs, 2 samples(cornus fruit, cnidium) were detected pesticides unnotificated MRLs.

• Journal of Food Hygiene and Safety
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• v.28 no.1
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• pp.13-18
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• 2013

This study was conducted to monitor residual pesticides in ginseng and balloon flower roots and to assess their risk to human health. All of 112 samples consisted of ginseng and balloon roots were purchased from traditional domestic markets and supermarkets in nine provinces of Korea in 2012. Multi-residue analysis of 122 pesticides was conducted and the analysis was performed by gas chromatography-electron capture detector, gas chromatography- nitrogen/phosphorus detector, and high-performance liquid chromatography. Seven pesticides were detected in 12 root samples and the detection rate was 10.7%. The detected twelve root samples were 10 ginseng root samples and 2 balloon root samples. Pesticides detected in root samples were procymidone, kresoxim-methyl, endosulfan, cypermethrin, tralomethrin, tetraconazole and chlorfluazuron. Among them, two pesticides as tetraconazole in a balloon flower root and cypermethrin in a ginseng root exceeded the recommended maximum residue limit set by Korea Food and Drug Administration. Five pesticides detected from 10 root samples were identified as unregistered pesticides in Korea. In order to do risk assessment with Korean medicinal plant consumption, estimated daily intake of residual pesticides were determined and compared to acceptable daily intake, referring to %ADI values. The range of %ADI values was from 0.006% to 0.333%. Taken together, it demonstrates the pesticides found in the two root samples were below the safety margin, indicating no effect on human health.

• 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.

• Journal of agriculture & life science
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• v.45 no.5
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• pp.73-80
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• 2011

Fifty substances of pesticide were selected for analysis through the historical investigation of pesticides detected from environmental-friendly agricultural soil, and the environmental-friendly agricultural soils in Gyeongnam area were collected and then were accepted Anve (accelerated solvent extraction) and SPve (solid-phase extraction) as multiresidue extraction and clean up methods suitable to the soils. The pesticide residues were analyzed by using GC/vCD/NPD, HPLC/UV/FL, GC/MSD, or HPLC/MSD. 50 kinds of pesticides for the soils were an average of 95.5% from retrieval ratio of the 72 to 118% range, and the average of 3.0% for CV (%). Among 40 samples of soil, 20 components were detected from pesticide residues of 21 samples, and average amounts detected for these components were 0.035 for endosulfan, 0.043 for ethoprophos, 0.020 for chlorpyrifos, 0.023 for chlorfenapyr, 0.047 for flufenoxuron, 0.070 for fenvalerate, 0.266 for cypermethrin, 0.016 for lufenuron, 0.022 for bifenthrin, 0.025 for fenobucarb/BPMC, 0.043 for difenoconazole, 0.059 for fenarimol, 0.020 for kresoxim-methyl, 0.026 for tetraconazole, 0.039 for isoprothiolane, 0.017 for iprobenfos, 0.014 for nolrimol, 0.156 for fluquinconazole, 0.047 for tebuconazole, and 0.045 mg/kg for oxadiazon. Therefore it is infered that the establishment of pesticide residues limit for environmental-friendly agricultural soil is needed as soon as possible.