• Title/Summary/Keyword: Pesticide analysis

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Monitoring of Residual Pesticides in Agricultural Products by LC/MS/MS (LC/MS/MS를 이용한 국내 유통 농산물의 잔류농약 실태조사)

  • Kim, Mi-Ok;Hwang, Hye-Shin;Lim, Moo-Song;Hong, Jee-Eun;Kim, Soon-Sun;Do, Jung-Ah;Choi, Dong-Mi;Cho, Dae-Hyun
    • Korean Journal of Food Science and Technology
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    • v.42 no.6
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    • pp.664-675
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    • 2010
  • This survey was carried out to estimate pesticide residue levels in commercial agricultural products in the year 2009. Residues were examined in 16 commodities (rice, foxtail millet, buckwheat, kidney beans, peanuts, sesame, oranges, grapefruit, kiwifruit, spinach, perilla leaves, leeks, garlic stem, garlic, ginger, and oak mushroom) collected from 22 provinces in Korea. Analyses were performed by multi-methods capable of detecting up to 60 pesticides by LC/MS/MS. A total of 510 samples were collected and analyzed. Of the samples, 96.1% contained no detectable pesticide residues. Detectable residues at or below the MRLs were found in 3.5% of the samples. However, in 0.4% of the samples (spinach and leeks), residue (ethaboxam and fluquinconazole) levels exceeded the MRLs. Furthermore, intake assessments of 7 kinds of pesticide residues were carried out, excluding those exceeding the MRLs. The results showed that the ratios of EDI (estimated daily intake) to ADI (acceptable daily intake) were 0.0001-0.0006%, which indicates that the detected pesticide residues were in a safe range. It is concluded that residual pesticides in agricultural products are properly controlled in Korea.

Analysis of Pesticides in Herbal Medicine by QuEChERS and GC-MS/MS (QuEChERS 전처리와 GC-MS/MS를 활용한 생약의 잔류농약 분석 가능성 연구)

  • Seo, Go Eun;Kim, A Young;Pyo, Byoung Sik;Lee, Kyoung in
    • Korean Journal of Pharmacognosy
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    • v.51 no.3
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    • pp.207-216
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    • 2020
  • The analysis method for qualitative analysis of the screening method that can be performed prior to the quantitative analysis of individual pesticide was reviewed in order to meet the safety standards that are being strengthened in the field of pesticide residue testing of herbal medicines. Among the residual pesticides presented in the Korean Pharmacopoeia, 56 pesticides, excluding 15 pesticides that need to be individually analyzed, were selected for analysis using QuEChERS preprocessing and GC-MS/MS, which are used in the existing agricultural products field. For each pesticide, the detection limit level of 0.001-0.005 mg/kg and the quantitative limit level of 0.002-0.017 mg/kg were confirmed. In the recovery test in which the standard was treated at a concentration of 0.02 mg/kg, it was confirmed that the proportion of pesticides satisfying the recovery of 70-120% was 85.7-96.4% for each herbal medicine, so it was confirmed that it was a level that could be reviewed by the screening method.

Monitoring and Risk Assessment of Pesticide Residues in Commercial Environment Friendly Fruits and Fruiting Vegetables (유통 친환경 과실류와 과채류 중 농약잔류 실태조사 및 안전성 평가)

  • Lee, Jae Yun;Noh, Hyun Ho;Park, So Hyun;Lee, Kwang Hun;Park, Hyo Kyoung;Hong, Su Myeong;Kim, Doo Ho;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.308-314
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    • 2012
  • In order to monitor the residual pesticides in environment friendly agricultural commodities, fruits and fruiting vegetables. Twenty-five agricultural commodities were collected twice in May and August 2011 from nine environment friendly agricultural commodities-selling supermarkets and retail stores located in eight major cities in Korea. The number of each agricultural commodity collected, 555 samples in total, was 152 organic agricultural products, 202 pesticide-free agricultural products and 201 low-pesticide agricultural products. Pesticide residues in samples were analyzed by multiresidue method for 245 pesticides using a GC-ECD/NPD and an HPLC-DAD/FLD and the peaks suspected as pesticides were identified with a GC/MSD. As a result of pesticide residue analysis, three pesticides, bifenthrin, EPN and chlorpyrifos, were detected from four samples including apple, representing a detection rate of 0.72%. The residue levels of the four pesticide-detected samples were less than their maximum residue limits (MRLs) but one pesticide EPN detected from pear exceeded its legible criterion of one twentieth MRL. Estimated daily intakes of the pesticides detected from fruits and fruiting vegetables were less than 0.76% of their maximum permissible intake.

Sensing of the Insecticide Carbofuran Residues by Surface Plasmon Resonance and Immunoassay (표면플라즈몬공명과 효소면역분석법을 이용한 살충제 카보후란 잔류물 검출)

  • Yang G. M.;Cho N. H.
    • Journal of Biosystems Engineering
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    • v.30 no.6 s.113
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    • pp.333-339
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    • 2005
  • The pesticide is raising public interest in the world, because it causes damage to an environmental pollution and the human health remaining agricultural products and an ecosystem, in spite of the advantages. Particularly, each country restricts the residual pesticide and induces observance about the safety and usage standard so that they can control the amount of pesticide used and defend the safety of agricultural products. The habitual practice for the analysis of the residual pesticide depends on GC (gas chromatography), HPLC (high performance liquid chromatography) and GC/MS (gas chromatography/mass spectroscopy), which triturate the fixed quantity of samples, abstract and purify as a suitable organic solvent. These methods have the highly efficient in aspects of sensitivity and accuracy. On the other hand, they need the high cost, time consuming, much effort, expensive equipment and the skillful management. Carbofuran is highly toxic by inhalation and ingestion and moderately toxic by dermal absorption. As with other carbamate compounds, it is metabolized in the liver and eventually excreted in the urine. The half-life of carbofuran on crops is about 4 days when applied to roots, and longer than 4 days if applied to the leaves. This research was conducted to develop immunoassay for detecting carbofuran residue quickly on the basis of surface plasmon resonance and to evaluate the measurement sensitivity. Gold chip used was CM5 spreaded dextran on the surface. An applied antibody to Immunoassay was GST (glutathione-s-transferase). The association and the dissociation time were 176 second and 215 second between GST and carbofuran. The total analysis time using surface plasmon resonance was 13 minutes including regeneration time, on the other hand HPLC and GC/MS was 2 hours usually. The minimum detection limit of a permissible amount for carbofuran in the country is 0.1 ppm. The immunoassay method using surface plasmon resonance was 0.002 ppm.

Monitoring and Safety Assessment of Pesticide Residues in Ginseng (Panax ginseng C.A. Meyer) from Traditional Markets (유통 수삼 중 잔류농약 모니터링 및 안전성 평가)

  • Noh, Hyun Ho;Lee, Jae Yun;Park, Hyo Kyoung;Jeong, Hye Rim;Lee, Jeong Woo;Jin, Me Jee;Choi, Hwang;Yun, Sang Soon;Kyung, Kee Sung
    • The Korean Journal of Pesticide Science
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    • v.20 no.1
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    • pp.23-29
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    • 2016
  • This study was carried out to survey residual characteristics of pesticide in fresh ginsengs collected from 45 markets at 15 regions in Korea using multiresidue analysis with a GC-MS/MS and an LC-MS/MS. After residue analysis was performed, the pesticides detected from ginsengs were quantitated using their analytical methods validated by recovery tests with a GC-ECD/NPD. As a results of analysis of pesticide residue, cypermethrin, fenitrothion, fludioxonil, thifluzamide, and tolclofos-methyl were detected from 16 samples among 45 samples in total, indicating detection rate was 35.6%. Tolclofos-methyl was found to be highest in detection frequency in ginseng. Fenitrothion that has not established maximum residue limit and pre-harvest interval for ginseng was detected. The amounts of all pesticides detected were less than their MRLs. Ratios of estimated daily intakes to acceptable daily intakes of the detected pesticides in ginseng were found to be from 0.03 to 16.67%.

Development of an Official Analytical Method for Determination of Imazapyr in Agricultural Commodities using HPLC-UVD (HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립)

  • Jang, Jin;Kim, Heejung;Ko, Ah-Young;Lee, Eun-Hyang;Joo, Yoon Ji;Kim, Jinhong;Chang, Moon-Ik;Rhee, Gyu-Seek
    • The Korean Journal of Pesticide Science
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    • v.19 no.1
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    • pp.5-13
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    • 2015
  • A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

Analysis of Kasugamycin in Pesticide Formulations by Reversed-Phase Ion Pair Liquid Chromatography (역상 이온쌍 액체크로마토그래피에 의한 농약 제품 중 Kasugamycin의 분석)

  • Kim, Taek-Jae;Kim, Kyong-Sun;Yoon, Chae-Hyuk;Joo, Jin-Bok;Kim, Chung-Hyo
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.343-349
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    • 1997
  • Analytical method using the reversed phase ion-pair chromatography (RP-IPC) for the determination of kasugamycin(5-amino-2-methyl-6-(2,3,4,5,6-pentahydroxy cyclohexyloxy)tetrahydropyran-3-yl-amino-${\alpha}$-imino acetic acid), pesticide as fungicide bactercide has been established. The retention behavior of kasugamycin in the RP-IPC was examined with respect to the effect of concentrations of organic modifiers, pH of eluent and types and concentrations of the counter ions as ion-pair reagent. This method developed by the optimum factors, can be used for the application of the quality control in the crude product and its formulation.

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Esophageal Cancer, Gastric Cancer and the use of Pesticides in the Southwestern of Turkey

  • Yildirim, Mustafa;Kaya, Vildan;Yildiz, Mustafa;Demirpence, Ozlem;Gunduz, Seyda;Dilli, Utku Donem
    • Asian Pacific Journal of Cancer Prevention
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    • v.15 no.6
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    • pp.2821-2823
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    • 2014
  • Background: Esophageal and gastric cancer generally have a poor prognosis and may share common risk factors. It has been demonstrated that the pesticide usage may contribute to development of many cancer types. In this study, the relation between amount of pesticides used in agriculture and esophageal and gastric cancer incidence was researched. Materials and Methods: Findings from the data bank of the Ministry of Health Provincial Health Directorate Cancer Records Center between the years of 1998-2010 were used. All patients who were diagnosed with gastric and esophageal cancer histopathologically were included. Data for annual pesticide usage were obtained from Provincial Agriculture Directorate for the same time period. Statistical analysis was performed using the Spearman test. Results: One thousand eight hundred and ninety-six patients were involved in the study, 1,233 males (65%) and 663 females (35%), 230 with esophageal cancer (12.1%) and 1,666 with gastric cancer (87.9%). No statistically significant relation was apparent between pesticide amount used and esophageal cancer (p: 0.87). Conclusions: In our study, there was no relationship between pesticide usage and esophageal or gastric cancer. However, the time between pesticide usage and cancer development was not known, qualifying the comparison.

Rapid Analysis of Tetraconazole Residues in Fruits and Vegetables using Ethyl Acetate Extraction and Gas Chromatography-tandem Mass Spectrometry

  • Xu, Jun;Dong, Fengshou;Liu, Xingang;Li, Jing;Li, Yuanbo;Shan, Weili;Zheng, Yongquan
    • Bulletin of the Korean Chemical Society
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    • v.32 no.12
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    • pp.4265-4269
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    • 2011
  • A method based on ethyl acetate extraction and gas chromatography with tandem mass spectrometry was developed for determining tetraconazole residues in fruits and vegetables. A 10 g homogenized sample was mixed with 10 mL ethyl acetate, shaken vigorously for 3 min, stored at $-20^{\circ}C$ for 15 min, and then vortexed vigorously for 1 min; 1 g NaCl and 4 g anhydrous $MgSO_4$ were added. The clean-up was carried out by applying dispersive solid-phase with 150 mg $MgSO_4$and 50 mg primary secondary amine. Three precursor product ion transitions for tetraconazole were measured and evaluated to provide the maximum degree of confidence. Average recoveries in fruits and vegetables at three levels (0.005, 0.05 and 0.5 mg/kg) ranged from 85.53% to 110.66% with relative standard deviations ($RSD_r$) from 1.3% to 17.5%. The LODs ranged from 0.002 to 0.004 ${\mu}g$/kg, and LOQs ranged from 0.006 to 0.012 ${\mu}g$/kg. This method was also applied to determine tetraconazole residue in cucumber dissipation experiment under field conditions. The half-lives of tetraconazole in cucumber were in the range of 2.1-3.1 days.

Pesticide Poisoning Deaths Detected at the National Forensic Service Headquarters in Seoul of Korea: A Five-Year Survey (2005-2009)

  • Lee, Sang-Ki;Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun
    • Environmental Analysis Health and Toxicology
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    • v.25 no.4
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    • pp.263-271
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    • 2010
  • Objectives : The records of 447 pesticide poisoning deaths from the National Forensic Service (NFS) headquarters located in Seoul of Korea from 2005 to 2009 were retrospectively reviewed. Methods : The data of each case were analyzed by using the SPSS program. Results : The mean age was $57.8{\pm}14.8$ years and the range was 16-92 years. The numbers of deaths of males and females were 301 and 134, respectively. The largest number of cases occurred in people aged 50-59 years (n=92, 20.6%) followed by the age groups 40-49 years (n=91, 20.4%), 60-69 years (n=88, 19.7%), and 70-79 years (n=75, 16.8%). The total number of deaths among other age groups (10-19, 20-29, 30-39, 80-89, and 90-99 years) was 73, representing only 16.3%. Of all pesticide poisoning deaths, 96.2% were due to suicide, and 28.4% of the total number who died received medical treatment. The mostfrequent site of ingestion was the person's own residence (n=279, 62.4%). The most common classes of pesticide were bipyridylium herbicide (paraquat, 31.1%), organophosphate insecticide (21.7%), and carbamate insecticide (15.4%). The major pesticides having a high proportion of fatalities were paraquat (31.1%), methomyl (11.4%), glyphosate (9.1%), dichlorvos (5.6%), phosphamidon (4.6%), and methidathion (4.0%). Conclusions : This study showed that poisoning deaths due to pesticides are one of the major public health problems in Korea. Enforcement of regulations and safety education to prevent pesticide poisoning should be carried out by the government.