• Title/Summary/Keyword: multiresidue method

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A Survey on Pesticide Residues of Commercial Agricultural Products in Gwangju Area (광주지역 유통 농산물의 농약 잔류실태 조사연구)

  • Kim Jongpil;Gang Gyunglee;Yang Yongshik;Lee Hyanghee;Chung Jaekeun;Kim Eunsun
    • Journal of Food Hygiene and Safety
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    • v.20 no.3
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    • pp.165-174
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    • 2005
  • This survey was conducted to monitor the current status of pesticide residues in agricultural products collected in wholesale markets and big retailers in Gwangju, in 2004. A total of 751 samples was analyzed by multiresidue method. Vegetables and fruits accounted for the largest proportion of the commodities analyzed and those two commodity groups comprised 604 $(80\%)\;and\;83\;(11\%)$ of the total number of 751 samples. Of these 751 samples, 112 samples $(14.9\%)$ had pesticide residues and 29 samples $(3.9\%)$ had violative residues. The detection rate was the highest $25\%$ in January and the lowest $9.5\%$ in June. The violation rate was the highest $7.0\%$ in March and the lowest $0\%$ in April. The violation rate in wholesale products was higher than that in big retailer products, $5.8\%$ verses $3.5\%$. And of 112 samples with pesticide residues, the agricultural product in which the pesticide residues were the most flequently detected was perilla leaf $(17.9\%)$ followed by korean lettuce $(16.1\%)$, spinach $(8.0\%)$ and korean cabbage $(5.4\%)$ and among 112 samples, 22 samples $(20\%)$ had more than one pesticide. Procymidone $(20.3\%)$, endosulfan $(18.2\%)$, dimethomorph $(13.3\%)$, chlorpyrifos $(7.7\%)$ and azoxystrobin $(6.3\%)$ were the most frequently found in agricultural product analyzed.

Gas Chromatographic Method for Multiresidue Analysis of Unregistered Pesticides in Imported Agricultural Commodities (가스 크로마토그래피를 이용한 수입농산물 중 국내 미등록 농약의 다성분 동시분석법 적용)

  • Lee, Ji-Won;Kang, Jeong-Kyun;Kwon, Hyeyoung;Ro, Jin-Ho;Jin, Yong-Duk;Lee, Je Bong;Hong, Su-Myeoung;Kim, Teak-Kyum;Cho, Nam-Jun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.161-173
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    • 2015
  • The multiresidue method 4.1.2.2 in Korea Food Code was extended for the analysis of 24 unregistered pesticide residues. The method includes acetonitrile extraction, liquid-liquid partition, Florisil SPE clean-up and GC analysis. The limits of quantification (LOQ) range of the method was 0.02~0.05 mg/kg for orange, brown rice and banana. The linearity for targeted pesticides were $R^2$ > 0.99 at the level ranged from 0.05 to 5 mg/L. Recovery test was performed at two concentration levels of LOQ and 4~10 times of LOQ. Recoveries and relative standard deviations (RSDs) of target pesticides were acceptable, showing 70~120% range and less than 20%, respectively, except for ethiprole, picloram and sulcotrion. This method is effectively applicable to routine analysis of target pesticides in orange, brown rice and banana.

Analysis of Diflubenzuron in Agricultural Commodities by Multiresidue Method (동시 다성분 분석법에 의한 농산물 중 Diflubenzuron 분석)

  • Park, Sun-Hee;Han, Chang-Ho;Kim, Ae-Kyung;Shin, Jae-Min;Lee, Jae-Kyoo;Park, Young-Hae;Kim, Ji-Min;Hwang, Lae-Hong;Chang, Min-Su;Song, Mi-Ok;Park, Ju-Sung;Yun, Eun-Sun;Kim, Mu-Sang;Jung, Kweon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.269-277
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    • 2014
  • The multiclass pesticide multiresidue method for the simultaneous determination of diflubenzuron in agricultural products was conducted by using HPLC-UVD. The method was validated through the guidelines of linearity, specificity, limit of detection (LOD), limit of quantification (LOQ), accuracy and precision with pesticide-free spinach, Korean cabbage, eggplant, squash, sweet pepper, cucumber, Korean melon. The calibration curve of diflubenzuron was linear over the concentration range of 0.05-5 mg/kg with correlation coefficient of above 0.99999. The limit of detection and quantification was 0.008 and 0.02 mg/kg. Mean recoveries of diflubenzuron for each sample were 77.5-105.6%. Relative standard deviation (RSD) in recoveries were all less than 20%. The intra-day and inter-day precision (RSD) were 0.4-1.9% and 0.7-1.9%, respectively. The result of validation indicated that this method was accurate and rapid assay.

Multiresidue Determination of Quinolones in Porcine, Chicken, and Bovine Muscle Using Liquid Chromatography with Fluorescence Detection

  • Lee, Sang-Hee;Shim, You-Sin;Kim, Hyun-Ju;Shin, Dong-Bin
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.978-984
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    • 2009
  • An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.

Multiresidue analytical method of pesticides in rice by HPLC (HPLC를 사용한 쌀 중 잔류농약 동시분석법)

  • Choi Jae-Chun;Lee Young-Ja;Kim So-Hee;Choi Soo-Young;Choi Hee-Ju;Jeong Seong-Wook;Park Heung-Jai;Kim Woo-Sung
    • Journal of Environmental Science International
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    • v.14 no.4
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    • pp.445-449
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    • 2005
  • A simple and sensitive analytical method based on RP-HPLC with UV detector$(225{\cal}nm)$ and mobile phases using $0.1{\%}$ phosphoric acid and acetonitrile was developed for simultaneous determination of quinclorac, bentazone, 2,4-D, bensulfuron-methyl, dymuron, capropamide, pencycuron, ethofenprox. This method was resulted in recovery of $78{\~}96{\%}$ with RSD $3.3{\~}7.5{\%}$, LODs $0.12{\~}0.84$ and LOQs $0.34{\~}1.20{\cal}mg/L$. Calibration curves were linear with r of $0.9995{\~}0.9999$.

A Survey on Pesticide Residues of Imported Agricultural Products Circulated in Gwangju (광주지역에서 유통되고 있는 수입 농산물의 잔류농약 실태조사)

  • Yang Yong-Shik;Seo Jung-Mi;Kim Jong-Pil;Oh Mu-Sul;Chung Jae-Keun;Kim Eun-Sun
    • Journal of Food Hygiene and Safety
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    • v.21 no.2
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    • pp.52-59
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    • 2006
  • This survey was conducted to monitor the current status of pesticide residues in imported agricultural products circulated in Gwangju, 2005. A total of 108 samples was analyzed by multiresidue method. Of these samples, 32 were citrus fruits, 60 were tropical fruits and grapes, and 16 were vagetables. The origin was Philippine for 39 samples, U.S.A. for 36, China for 12, New Zealand for 11, Chile for 6, etc. The overall rate of detections was 30.6% and no samples had violative residues. Of citrus fruits,20 samples (62.5%) had residues and the residues were thiabendazole, imazalil, chlorpyrifos, etc. Of tropical fruits and grapes, 13 samples (12.0%) had residues and the residues were azoxystrobin, chlorpyrifos, carbendazim, captan, etc. 16 of vagetables had no detectable pesticide residues. Thiabendazole (71% in oranges and 56% in grapefruits) and imazalil (50% in oranges) were found in citrus fruits, which were frequently used as post-harvest pesticides. And azoxystrobin which is one of strobilurin fungicides, was often detected in mango, tropical fruit(27%).

Multiresidue Analysis of 124 Pesticides in Soils with QuEChERS extraction and LC-MS/MS (QuEChERS 및 LC-MS/MS를 이용한 토양 중 124종 잔류농약다성분 분석법)

  • Gwon, Ji-Hyeong;Kim, Taek-Kyum;Seo, Eun-Kyung;Hong, Su-Myeong;Kwon, Hye-Yong;Kyung, Ki-Sung;Kim, Jang-Eok;Cho, Nam-Jun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.296-313
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    • 2014
  • A QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) multiresidue method was developed for the simultaneous analysis of 124 pesticides in soil by LC-MS. The procedure involved liquid extraction of soil immersed with 0.2N $NH_4Cl$ by acetonitrile with 1% acetic acid, followed by anhydrous $MgSO_4$ and sodium acetate, and dispersive SPE cleanup with $MgSO_4$, primary secondary amine (PSA) and $C_{18}$. The extracts were analyzed with LC-MS/MS in ESI positive mode. Standard calibration curves were made by matrix matched standards and their correlation coefficients were higher than 0.99. Recovery studies for the validation were carried out using two type soils, loam and sandy loam, at four concentration levels (0.005, 0.01, 0.02, and 0.1 mg/kg). The recoveries of pesticides were in the range of 70-120% with < 20% RSD except 4 pesticides, Benfuracarb, Ethiofencarb, Pymetrozine, and Pyrethrin. This result indicated that the method using QuEChERS and LC-MS/MS could be applied for the simultaneous determination of pesticide residues in soils.

Survey on Pesticide Residues in Commercial Agricultural Products in the Northern Area of Seoul (서울특별시 강북지역 유통 농산물들에 대한 농약잔류실태조사)

  • Seung, Hyun-Jung;Park, Sung-Kyu;Ha, Kwang-Tae;Kim, Ouk-Hee;Choi, Young-Hee;Kim, Si-Jung;Lee, Kyeong-Ah;Jang, Jung-Im;Jo, Han-Bin;Choi, Byung-Hyun
    • Journal of Food Hygiene and Safety
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    • v.25 no.2
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    • pp.106-117
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    • 2010
  • This study was carried out to investigate the current status of pesticide residues in 3,988 agricultural products in the northern area of Seoul from January to December in 2009. 3,988 samples comprising 109 types of agricultural products were assessed via a multiresidue method to detect 272 pesticides. Pesticide residues were detected in 25.6% (1,021 of 3,988 samples), and the rate at which the detected residues violated the maximum residue levels (MRLs) of the Korean Food Code was 2.2% (89 of 3,988 samples). The agricultural products which exceeded their maximum residue limits were leek, ginseng, welsh onion, crown daisy and lettuce (leaf). Additionally, the most frequently detected pesticide that exceeded the regulation maximum was endosulfan, procymidone, tolclofos-methyl, iprodione and flutolanil.

Research on Pesticides Residue in Commercial Agricultural Products in 2009 (2009년 유통 농산물 중 잔류농약 실태조사)

  • Lee, Ju-Young;Choe, Won-Jo;Lee, Hee-Jung;Shin, Yong-Woon;Do, Jung-Ah;Kim, Woo-Seong;Choi, Dong-Mi;Chae, Kab-Ryong;Kang, Chan-Soon
    • Journal of Food Hygiene and Safety
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    • v.25 no.2
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    • pp.192-202
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    • 2010
  • Pesticide residues were investigated in 16 commodities (rice, foxtail millet, buckwheat, kidney bean, peanut, sesame, orange, grapefruit, kiwifruit, spinach, perilla leaves, leek, garlic stem, garlic, ginger and oak mushroom) collected from 22 provinces (Seoul, Busan, Incheon, Daegu, Daejeon, Gwangju, Ulsan, Suwon, Seongnam, Goyang, Bucheon, Yongin, Cheongju, Jeonju, Jeju, Cheonan, Changwon, Pohang, Gumi, Jinju, Wonju and Yeosu) in 2009. Pesticides (172 kinds) were analyzed using multiresidue method by GC/MS/MS from 510 samples, and phenthoate in kiwifruit was violated by exceeding MRL. The intake assessment for 24 kinds of pesticide residues including the detected pesticides at multi pesticide residue monitoring (bifenthrin etc.) were carried out. The result showed that the ratio of EDI (estimated daily intake) to ADI (acceptable daily intake) was 0.000007~0.458% which means that the detected pesticide residues were in a safe range so that residual pesticides in the agricultural products in Korea.

A Study on the Pesticide Residues Monitoring of Medicinal Herbs which has marketed in the Daejeon (대전 지역 유통 식용 한약재의 잔류농약 실태 연구)

  • Kim, Kyoung-Shin;Kim, Sung Gu;Lim, Jae Yeun;Kim, Byoung-Soo
    • Journal of Haehwa Medicine
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    • v.22 no.1
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    • pp.129-143
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    • 2013
  • This study was conducted to investigate the residue amount of pesticide on the 41 medicinal herbs in Daejeon area. This study was carried out to monitor the current status of pesticide residues in commercial medicinal herbs for sale of food use in 2012. It was performed using GC/ECD, GC/NPD, HPLC to analyze pesticides residues. Residues of 283 pesticides were analyzed by a simultaneous multiresidue method in 41 medicinal herbs being on sale in Daejeon. The medicinal herbs detected pesticides in 10 of 41 cases, showed a detection rate of 24.39%. The medicinal herbs which exceed the maximum residue limit were five cases as Cnidii Rhizoma, Osterici Radix, Artemisiae Capillaris Herba, Zizyphi Fructus and Alismatis Rhizoma. And pesticide residue of Cnidii Rhizoma and Alismatis Rhizoma exceeds the limit standard presented in only medicine use of KFDA. The residual pesticides which had the high detection rate were Chlopyrifos, Tebuconazole and Endosulfan in the detection of medicinal herbs. For further research, standards of Pesticide Residues in medicinal herbs should be added and more research of pesticide residues in medicinal herbs required. And standards of pesticide residues in medicinal herbs should be applied equally as medicines and food.