• Title/Summary/Keyword: multi-pesticide residue

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Multiresidue Analysis of 240 Pesticides in Apple and Lettuce by QuEChERS Sample Preparation and HPLC-MS/MS Analysis (QuEChERS 전처리법과 HPLC-MS/MS 기기분석을 이용한 사과와 상추 중 240종 농약의 동시분석)

  • Kwon, Hye-Young;Kim, Chan-Sub;Park, Byung-Jun;Jin, Yong-Duk;Son, Kyung-Ae;Hong, Su-Myeong;Lee, Je-Bong;Im, Geon-Jae
    • 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.

A Survey on the Residual Pesticides on Agricultural Products on the Markets in Incheon from 2016 to 2018 (인천광역시 유통 농산물의 최근 3년간 잔류농약 실태조사)

  • Park, Jeong-Eun;Lee, Mi-Yeon;Kim, Sun-Hoi;Song, Sung-Min;Park, Byung-Kyu;Seo, Soon-Jae;Song, Jae-Yong;Hur, Myong-Je
    • Korean Journal of Environmental Agriculture
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    • v.38 no.3
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    • pp.205-212
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    • 2019
  • BACKGROUND: This survey conducted on agricultural products in Incheon for the past three years from 2016 to 2018 to detect residual pesticides and to monitor the use of pesticides. METHODS AND RESULTS: Residual pesticides were analyzed for a total of 5,937 agricultural products in Samsan wholesale market, traditional market and large retailers in Incheon. Samples were analyzed by multi class pesticide method using GC-MS/MS, LC-MS/MS, GC-ECD/NPD, and UHPLC. In 59 cases (1.0%) residual pesticides were detected improperly and these cases exceeded maximum residue limits (MRLs). CONCLUSION: The ratios of violative agricultural products were similar each year at approximately 1.0% per year, but the residual pesticide detection rates with the limit included in the samples were shown to be gradually decreasing to 17.9%, 12.6%, and 11.2% annually. The frequency of violative residual pesticides was high in order of Diazinon, Chlorpyrifos, Iprodione, etc. Residual pesticide monitoring might be needed in the future continuously, as violations in agricultural products distributed in Incheon are shown at a similar level every year.

Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method (곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발)

  • Yang, In-Cheol;Hong, Su-Myeong;Kwon, Hye-Young;Kim, Taek-Kyum;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.314-334
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    • 2013
  • This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Monitoring and risk assessment of pesticide residues in school foodservice agricultural products in Incheon (인천광역시 학교급식 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Park, Byung-Kyu;Kwon, Sung-Hee;Yeom, Mi-Sook;Han, Se-Youn;Kang, Min-Jung;Seo, Soon-Jae;Joo, Kwang-Sig;Heo, Myung-Je
    • Korean Journal of Food Science and Technology
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    • v.53 no.4
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    • pp.470-478
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    • 2021
  • This study was conducted to monitor residual pesticides in a total of 527 school foodservice agricultural products from 2019 to 2020 in Incheon. Pesticide residues in the samples were analyzed by the multi-residue method in the Korean food code for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD, and HPLC-UVD. By monitoring the pesticides, 12 (2.3%) of the 527 pesticides were detected, and 2 (0.4%) samples exceeded the maximum residue limit. Twelve types of pesticides were detected in the agricultural products of carrot, chard, chili pepper, chwinamul, crown daisy, parsley, perilla leaves, and spinach. As a means of risk assessment through the consumption of agricultural products detected with pesticide residues, the proportion of estimated daily intake to acceptable daily intake was estimated in the range of 0.0000-39.7425%. Results showed no particular health risk through the consumption of school foodservice agricultural products with pesticide residues.

Monitoring and Risk Assessment of Pesticide Residues in School Foodservice Agricultural Products in Gwangju Metropolitan Area (광주광역시 학교급식 농산물의 잔류농약 모니터링 및 위해평가)

  • Kim, Jinhee;Lee, Davin;Lee, Mingyou;Ryu, Keunyoung;Kim, Taesun;Gang, Gyungri;Seo, Kyewon;Kim, Jung-Beom
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.283-289
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    • 2019
  • This study was performed to monitor the residual pesticides in agricultural products used in school foodservice in the Gwangju metropolitan area. Risk assessment was also carried out based on the amount of agricultural products consumed. A total of 320 agricultural products supplied to schools in Gwangju were analyzed from 2015 to 2017. The pre-treatment and residual pesticide analysis of these products was conducted in accordance with the second method for multi-residue analysis of pesticides in the Korean food code. The hazard index was calculated by dividing the estimated daily intake (EDI) of pesticides by the acceptable daily intake (ADI). The linearity correlation coefficient for the calibration curve was 0.9923 to 1.0000, LOD 0.004 to 0.019 mg/kg, LOQ 0.012 to 0.057 mg/kg, and recovery was 79.1 to 100.2%. Residual pesticides were detected in 18 (5.6%) of 320 agricultural products used for school foodservice, and one sample of sweet potato stem (0.3%) exceeded the maximum residual limit (MRL). The detection frequency for chili peppers and bell peppers was higher than that for other agricultural products. The frequently-detected pesticides were boscalid and acetamiprid. These results showed that residual pesticide management is needed for chili pepper, bell pepper and sweet potato stem among agricultural products supplied to schools. The hazard index of bifenthrin in sweet potato stem showed the highest (64.18%), and the other pesticides were 0.03-8.23%. These results indicated that agricultural products supplied to schools in Gwangju were safe for consumption. To minimize the intake of residual pesticides, it is necessary to not only thoroughly wash agricultural products but to also ensure the expanded supply of products that are pesticide-free.

Monitoring of Pesticide Residues on Herbs and Spices (향신식물의 잔류농약 실태조사)

  • Bae, Ho-Jeong;Kim, Woon-Ho;Jung, You-Jung;Lee, Yu-Na;Moon, Kyeong-Eun;Kim, Jung-Sun;Chae, Kyung-Suk;Lee, Jin-Hee;Do, Young-Sook;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.36 no.5
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    • pp.392-399
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    • 2021
  • This study was conducted to research the status of pesticide residues in a total of 114 herbs and spices obtained from January to October 2020. 341 pesticide residues were analyzed by the multi class pesticide multiresidue methods using GC-MSMS, GC-ECD, GC-NPD, LC-MSMS, LC-PDA, and LC-CAS. As a result of analysis, 36 pesticide residues were found, and detection rate was 31.6%. Of them, seven samples were detected over Maximum Residue Limits (MRLs) and the unsuitable level in pesticide was 6.1%. The herbs and spices exceeding MRLs include coriander (2 times), mint (2 times), basil (once), rosemary (once), and boraye (once). According to an analysis of 341 pesticide residues, 22 pesticides were detected 52 times and 8 pesticides were found to exceed the MRLs. The pesticides exceeding MRLs were ingredients such as etofenprox, flufenoxuron, fluquinconazole, iprodione, lufenuron, paclobutrazol, phenthoate, and spiromesifen.

Modified QuEChERS Multi-Residue Analysis Method for 61 pesticides in Fruits using with HPLC and GC-ECD/NPD (HPLC 및 GC-ECD/NPD를 이용한 과일 중 61종 농약의 QuEChERS 전처리 다성분 분석법 개발)

  • Lee, Ju-Young;Hong, Su-Myeong;Kim, Taek-Kyum;Min, Zaw Win;Kim, Yang-Hyeon;Song, Kyung-Ae;Kwon, Hye-Yong;Lee, Hee-Dong;Im, Geon-Jae;Kim, Doo-Ho;Kim, Jang-Eok
    • 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.

Development of Multi-residue Analysis and Monitoring of Persistent Organic Pollutants (POPs) - Used Organochlorine Pesticides in Korea (국내에 사용되어 금지된 유기염소계 농약류의 다중분석법과 모니터링)

  • Lim, Sung-Jin;Oh, Young-Tak;Yang, Ji-Yeon;Ro, Jin-Ho;Choi, Geun-Hyoung;Ryu, Song-Hee;Moon, Byeong-Chul;Park, Byung-Jun
    • The Korean Journal of Pesticide Science
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    • v.20 no.4
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    • pp.319-325
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    • 2016
  • This study was conducted to investigate residual organochlorine pesticides in green house soil and oriental melon, green pepper, and lettuce. The majority of them were designated as persistent organic pollutants (POPs) by the international community at the Stockholm Convention on Persistent Organic Pollutant. Extraction and clean-up method were developed using the QuEChERS method for residual organochlorine pesticides (OCPs) in soil and oriental melon, green pepper and lettuce. Recovery of OCPs in greenhouse soil and oriental melon, green pepper, and lettuce ranged from 73.3-110.6%. Limit of detection (LOD) of OCPs in soil and 3 crops were 0.01-0.08 and $0.11-0.17{\mu}g/kg$. The residues of OCPs in oriental melon, green pepper and lettuce greenhouse soil were analyzed by the developed method, and dieldrin, ${\beta}-endosulfan$ and endosulfan sulfate were detected at 1.4-72.5, 0.1-78.7 and $0.0-214.1{\mu}g/kg$, respectively. The detection frequency of 3 compounds in soils were 52 (29.7%), 34 (19.4%) and 57 (32.6%) among 175 samples, respectively. However, these compounds were not detected in all crop samples. The residue level in 3 crops were lower than 1/58.8 of maximum residue level of them. These results showed that the OCPs residue in oriental melon, green pepper, and lettuce greenhouse soil were not as high as crop safety threatening.

Monitoring and Risk Assessment of Pesticide Residues on Stalk and Stem Vegetables Marketed in Incheon Metropolitan Area (인천광역시 유통 엽경채류 농산물의 잔류농약 실태조사 및 위해성 평가)

  • Park, Byung-Kyu;Jung, Seung-Hye;Kwon, Sung-Hee;Ye, Eun-Young;Lee, Han-Jung;Seo, Soon-Jae;Joo, Kwang-Sig;Heo, Myung-Je
    • Journal of Food Hygiene and Safety
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    • v.35 no.4
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    • pp.365-374
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    • 2020
  • This study was conducted to monitor the residual pesticides on a total of 320 stalk and stem vegetables from January 2019 to December 2019 in the Incheon metropolitan area. Pesticide residues in samples were analyzed by the multi-residue method for 373 pesticides using GC-MS/MS, LC-MS/MS, GC-ECD, GC-NPD and HPLC-UVD. Risk assessment was also carried out based on the amount of stalk and stem vegetables consumed. The linearity correlation coefficient for the calibration curve was 0.9951 to 1.0000, LOD 0.002 to 0.022 mg/kg, LOQ 0.005 to 0.066 mg/kg and recovery was 82.0 to 108.0%. According to the monitoring of pesticides, 36 (11.3%) of 320 were detected with pesticide residues and 3 (0.9%) samples exceeded the maximum residual limit. The detection frequency for Chinese chives and Welsh onion was higher than that for other stalk and stem vegetables. The frequently detected pesticides were etofenprox, procymidone, fludioxonil, and pendimethalin. As a tool of risk assessment through the consumption of pesticide detectable agricultural products, the ratio of estimated daily intake (EDI) to acceptable daily intake (ADI) was calculated in the range of 0.0062-24.1423%. These results indicate that there is no particular health risk through consumption of commercial stalk and stem vegetables detected with pesticide residues.

Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).