• Title/Summary/Keyword: multi-residue pesticides

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Development of Multi-residue Analysis of 320 Pesticides in Apple and Rice Using LC-MS/MS and GC-MS/MS (LC-MS/MS와 GC-MS/MS를 이용한 사과와 쌀 시료에서 320종 농약의 다성분 분석)

  • Kim, Jong-Hwan;Kim, Yeong-Jin;Kwon, Young-Sang;Seo, Jong-Su
    • The Korean Journal of Pesticide Science
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    • v.20 no.2
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    • pp.104-127
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    • 2016
  • A new analytical method has been developed to determine 320 pesticides in apple and rice. The extraction of pesticides was carried out based on QuEChERS sample extraction, and determination was performed using LC-MS/MS and GC-MS/MS. 320 pesticides were selected for experiments. 251 and 110 pesticides among them were analysed by LC-MS/MS and GC-MS/MS, respectively. 41 pesticides of them were analyzed by both GC-MS/MS and LC-MS/MS. Among pesticides analysed by LC, 242 pesticides (96% of total number) in apple and 237 pesticides (94% of total number) in rice showed recoveries in the range of 70~120% with RSD ${\leq}20%$. In case of pesticides analyzed by GC-MS/MS, 103 pesticides (94% of total number) in apple and 83 pesticides (76% of total number) in rice were successfully validated. These results indicated that LC-MS/MS and GC-MS/MS analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in agricultural products.

Multi-Pesticide Residue Method for Analysis of Organochlorine and Organophosphorus Pesticide

  • Bonghun Lee;Woo
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 1997.10a
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    • pp.37-39
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

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A Safety Survey of Pesticide Residues in Fruit Products Circulated in Chungcheongnam-do Province, Korea (충남도내 유통 과일류의 잔류농약 안전성 조사)

  • Lee, Kang-Bum;Kim, Nam-Woo;Song, Nak-Soo;Lee, Jung-Ho;Jung, Sang-Mi;Shin, Myoung-Hee;Choi, Seon-Sil;Kim, Ji-Hee;Sung, Si-Youl
    • Journal of Food Hygiene and Safety
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    • v.34 no.5
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    • pp.421-430
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    • 2019
  • In this study, 195 pesticide residues in fruit samples (n=150) at local markets in Chungcheongnam-do Chungnam, Korea were monitored using a multi-residue method combined with GC-MS/MS and LCMS/MS. Among 150 fruit samples, 40 types of pesticides were detected in 63 samples and the detection rate was 42.0%. However, the amounts were below the maximum residue limit (MRL). Detection rates for pesticides in each thpe of fruit were as follows ; citrus fruits (55.2%), pome fruits (41.3%), berries (38.7%) and stone fruits (36.0%). Although the sample size was small (n=2), pesticide residues were not detected in tropical fruits. Occurrences of detection of pesticide residues in apple showed the highest level, and mainly, insecticides were detected most frequently. The most commonly detected pesticides residues were bifenthrin (21), pyraclostrobin (17), novaluron (13), boscalid (10), chlorfenapyr (9), trifloxystrobin (9), furathiocarb (9), acetamiprid (8) and chlorpyrifos (8). Five types of residual pesticides (bifenthrin, chlorfenapyr, deltamethrin, fenpropathrin and fenvalerate) were detected in quince, and out of these five, fenpropathrin exceeded the MRL based on the Positive List System (PLS). These results suggested that pesticide residues in fruit samples should be continuously monitored, although residue levels in 63 other fruit samples were evaluated as being within a safe level.

Gas Chromatographic Performances for Simultaneous Determination of Multi-pesticide Residues and Extraction of Pesticides with Three Partition Solvents (잔류농약 다성분 동시분석을 위한 기체 크로마토그래피 분석성능과 3종 분배용매에 의한 농약추출)

  • Kim, Chan-Sub;Kim, Jin-Bae;Im, Geon-Jae;Park, Hyun-Ju;Lee, Young-Deuk
    • The Korean Journal of Pesticide Science
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    • v.13 no.3
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    • pp.133-147
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    • 2009
  • In order to develop the simultaneous analytical method for pesticide residues which ones in soil are rapidly and inexpensively measured by, many analytical methods for individual pesticide residue and several methods for multi-pesticide residues in agricultural commodities and food were reviewed. Various gas chromatographic conditions and pre-treatment procedures were intensively investigated and modified. And then new optimum procedure was established and its proficiency was validated. The response on detectors of simultaneous determination of 180 pesticides out of pesticides used in Korea was tested. The number of pesticides that their limits of detection (LOD) equal or lower than $0.05\;mg\;kg^{-1}$ were 137 pesticides on ECD, 170 pesticides on NPD and 179 pesticides on ECD/NPD integrated. The retention times of most pesticides ranged appropriately between 10 minutes and 40 minutes in the proposed chromatographic conditions. But about 90 pesticides eluded between 20 minutes and 30 minutes and so they were not resolved enough. In partition with dichloromethane, ethyl acetate/hexane (1:1) and ethyl acetate, number of pesticides whose extraction efficiency ranged from 70% to 120%, were 163, 154 and 147, respectively.

Monitoring of Pesticide Residues and Risk Assessment for Medicinal Plants (국내 유통 약용식물 중 잔류농약 모니터링 및 위해성 평가)

  • Ahn, Ji-Woon;Jeon, Young-Hwan;Hwang, Jeong-In;Kim, Jeong-Min;Seok, Da-Rong;Lee, Eun-Hyang;Lee, Sung-Eun;Chung, Duck-Hwa;Kim, Jang-Eok
    • 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.

Development of Analytical Reference Material for Proficiency Test of Pesticide Multi-residue Analysis in Green-pepper (풋고추 농약다성분분석 정도관리용 분석표준물질 개발)

  • Kim, Jong-Hwan;Choi, Sung-Gil;Oh, Young-Gon;Kwon, Young-Sang;Hong, Su-Myeong;Sung, Mun-Hyun;Lee, Se-Ja;Hwang, Sun-Young;Seo, Jong-Su
    • The Korean Journal of Pesticide Science
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    • v.20 no.3
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    • pp.211-220
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    • 2016
  • This study was to develop the analytical reference material of green-pepper for multi-residue analysis of pesticides. According to the ISO Guide 35, ISO Guide 13528 and EURL-PT protocol, the homogeneity, stability, assigned value and uncertainty were calculated to assess if it was suitable to be used as the proficiency test or quality control. The values of the within-bottle standard variation ($s_{wb}$) and the between-bottle standard variation ($s_{bb}$) were 1.7~3.7% of assigned value according to the requirement of the ISO guide 35. And, the uncertainty ($u^*{_{bb}}$) due to inhomogeneity was 0.8~1.1% for all pesticides. The storage stabilities of ten-pesticides at various conditions were assessed. For all target pesticides, the slop ($b_1$) values were smaller than the corresponding values of $[t_{0.95,n-2}{\times}s(b_1)]$ specified by the ISO guide 35, indicating that there were no statistically significant decreases in the concentration of the target pesticides when the analytical reference material was stored at room temperature ($20{\sim}30^{\circ}C$) for 7 days, freezing ($-20^{\circ}C$) for 30 days and deep freezer ($-80^{\circ}C$. except for bifenthrin, fenpropathrin) for 245 days. For proficiency test by using it developed by Korea Institute of Toxicology, inter-lab test was performed with eight organization performing the residual pesticide analysis. We found that there were some different results among them. Some were assessed as questionable or unacceptable for two pesticides and one organization didn't analyze the six pesticides. From these results, this green-pepper analytical reference material containing ten-pesticides could be used as a tool for the proficiency test to improve the reliability or consistency for pesticide residue's results.

Establishment of Simultaneous Analysis Method for the Detection of Multi-Pesticide Residue Used in Golf Courses (골프장 농약 검사를 위한 다성분 동시분석방법 확립에 관한 연구)

  • Yun, Jeong-Ki;Lee, Min-Hyo;Noh, Hoe-Jung;Park, Jong-Gyum;Kim, Hyuk;Kim, Chan-Sub
    • Journal of Soil and Groundwater Environment
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    • v.11 no.4
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    • pp.18-24
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    • 2006
  • The possibility of multiresidue analysis of 24 pesticides out of 30 residual pesticides which are subjected to test in the golf courses was examined. The utility of multiresidue method for pesticide residue test was evaluated by recovery test through a standard addition method of pesticides in water, soil, and lawn grass. The experimental results of the recovery test for individual pesticides are as follows : The number of pesticide of which average recovery rate was over 70% regardless of media was 16 pesticides. These pesticides were composed of 8 organophosphorus pesticides (chlorpyrifos, chlorpyrifosmethyl, diazinon, EPN, fenitrothion, phenthoate, phosalone, and toclofos-methyl). 4-organochlorinated pesticides (daconil, captan, endosulfan, and tetradifon), 2-pyrethroid pesticides(fenpropathrin, lambda-cyhalothrin) and 2 other pesticides (bromopropylate, pendimethalin). On the other hand, in case of dicofol, average recovery rate was over 70% for water and lawn grass but only 53.3% for soil. Therefore, the multiresidue method applied in this experiment is not appropriate for analysis of dicofol in soil. Furthermore, among 7 pesticides, 2 pesticides(amitraz and pyraclofos) showed that theirs average recovery rate deviated from criteria($70{\sim}130%$) in almost ail media, while 5 pesticides(bensulide, deltamethrin, iprodione, phosphamidon and tralomethlin) were not detected from all media by GC/NPD or GC/ECD.

Research of pesticide residue of domestic Lentinula edodes related with the positive list system (농약 허용물질목록 관리제도와 연계한 국내산 표고 잔류농약 실태 조사)

  • Kim, Kyung-Je;Koh, Young-Woo;Im, Seung-Bin;Jin, Seong-Woo;Ha, Neul-I;Jeong, Hee-Gyeong;Jeong, Sang-Wook;Yun, Kyeong-Won;Seo, Kyoung-Sun
    • 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.

Multi-Pesticide Residue Method for Organopesticide Analysis (유기농약 분석을 위한 Multi-Pesticide Residue Method)

  • 김우성;이봉헌
    • Journal of Environmental Science International
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    • v.6 no.4
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    • pp.385-389
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC /ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pegticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azlnphos-methyls. The minimum detectable levels of this analytical method were low(0.021-0.058mg/kg).

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