• Title/Summary/Keyword: 잔류물질

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Studies on the Content and Heat Decomposition of Residual Tetracycline in Meats on the Market (시판 육류중의 Tetracycline계 항생물질 잔류량과 가열분해에 관한 연구)

  • 배기철;이영근
    • Journal of Food Hygiene and Safety
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    • v.6 no.2
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    • pp.83-87
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    • 1991
  • Beef, pork and chicken on the market were analyzed for determination of tetracyclines residue and decomposition of tetracyclines by heating were studied. The content of oxytetracycline was trace in chicken A, 0.09 mg/kg in C and trace in beef C, pork A and B, but in the other samples was not detected oxytetracycline. Chlortetracycline residue was 0.14, 0.02 and 0.01 mg/kg in chicken A, C and beef B respectively. In HPLC analysis, two peaks of 8.1 and 9.0 min of retention time were found from beef and pork and expected to be component of meat, and because of same retention time, the one of 9.0 min interrupted determination of tetracycline. But those were not found in chicken, therefore the residue was 0.01 mg/kg in sample A. The residue were degradated rapidly by heating of roast, but slightly by that of boiling.

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Determination and Validation of an Analytical Method for Dichlobentiazox in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증)

  • Gu, Sun Young;Lee, Han Sol;Park, Ji-Su;Lee, Su Jung;Shin, Hye-Sun;Kang, Sung Eun;Chung, Yun Mi;Choi, Ha Na;Yoon, Sang Soon;Jung, Young-Hyun;Yoon, Hae Jung
    • Korean Journal of Environmental Agriculture
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    • v.40 no.2
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    • pp.108-117
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    • 2021
  • BACKGROUND: Dichlobentiazox is a newly registered pesticide in Korea as a triazole fungicide and requires establishment of an official analysis method for the safety management. Therefore, the aim of this study was to determine the residual analysis method of dichlobentiazox for the five representative agricultural products. METHODS AND RESULTS: Three QuEChERS methods were applied to establish the extraction method, and the EN method was finally selected through the recovery test. In addition, various adsorbent agents were applied to establish the clean-up method. As a result, it was found that the recovery of the tested pesticide was reduced when using the d-SPE method with PSA and GCB, but C18 showed an excellent recovery. Therefore this method was established as the final analysis method. For the analysis, LC-MS/MS was used with consideration of the selectivity and sensitivity of the target pesticide and was operated in MRM mode. The results of the recovery test using the established analysis method and inter laboratory validation showed a valid range of 70-120%, with standard deviation and coefficient of variation of less than 3.0% and 11.6%, respectively. CONCLUSION: Dichlobentiazox could be analyzed with a modified QuEChERS method, and the method determined would be widely available to ensure the safety of residual pesticides in Korea.

Development and Validation of an Analytical Method for Quinoxyfen in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 살균제 Quinoxyfen의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.140-147
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    • 2019
  • An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with $MgSO_4$ (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using $MgSO_4$, PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels ($0.001-0.25{\mu}g/mL$) and the coefficient of determination ($R^2$) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

육류의 유해잔류물질 방지대책

  • Kim, Ok-Gyeong
    • The Korea Swine Journal
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    • v.12 no.10 s.134
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    • pp.42-45
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    • 1990
  • 보건사회부는 식품위생법에 따라 오는12월 1일부터 돼지고기,쇠고기,닭고기 등 유통육류에 대해 유해물질 잔류 검사를 실시할 계획이다

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Development and Validation of an Analytical Method for Fenpropimorph in Agricultural Products Using QuEChERS and LC-MS/MS (QuEChERS법과 LC-MS/MS를 이용한 농산물 중 Fenpropimorph 시험법 개발 및 검증)

  • Lee, Han Sol;Do, Jung-Ah;Park, Ji-Su;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Choi, Young-Nae;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.115-123
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    • 2019
  • An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.

Microplastic Management for Preventing Risk of Persistent/Bioaccumulative Substance (잔류성.생물축적성 물질 피해저감을 위한 미세플라스틱(Microplastic) 관리방안)

  • Park, Jeong-Gue;Gan, Sun-Yeong
    • Journal of Environmental Policy
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    • v.13 no.2
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    • pp.65-98
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    • 2014
  • Plastics of the marine environment are broken gradually down into smaller particles by chemical weathering, called "microplastic". Microplastics absorb organic pollutants that are persistent bioaccumulative substances. If marine animals ingested microplastic added to contaminant, it will lead to a bioaccumation through the food web. It eventually destroy health of marine environment and is harmful to marine top predators including humans. Also, Microplastics can impact marine animals by leaching the endocrine disruptor in microplastic itself as well as playing an adsorbent role of organic pollutants. Persistent and bioaccumulative substances in Korea have been regulated in terms of chemical risk but existing regulations largely have been limited in land-based source management of microplastic. Thus, the harmful impact will be increased whether the microplastics absorbed contaminants. To prevent risk of persistent bioaccumulative substances, this study suggests the following: (1) the strict management of microplastic by designating the hazardous substances, (2) expand the use of biodegradable plastic, (3) the effort for reuse and recycle, (4) the expand of microplastic clean-up programs.

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Selection and Validation of an Analytical Method for Trifludimoxazin in Agricultural Products with LC-MS/MS (LC-MS/MS를 이용한 농산물 중 Trifludimoxazin의 시험법 선정 및 검증)

  • Sun Young Gu;Su Jung Lee;So eun Lee;Chae Young Park;Jung Mi Lee;Inju Park;Yun Mi Chung;Gui Hyun Jang;Guiim Moon
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.79-88
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    • 2023
  • Trifludimoxazin is a triazinone herbicide that inhibits the synthesis of protoporphyrinogen oxidase (PPO). The lack of PPO damages the cell membranes, leading to plant cell death. An official analytical method for the safety management of trifludimoxazin is necessary because it is a newly registered herbicide in Korea. Therefore, this study aimed to develop a residual analysis method to detect trifludimoxazin in five representative agricultural products. The EN method was established as the final extraction method by comparing the recovery test and matrix effect with those of the QuEChERS method. Various sorbent agents were used to establish the clean-up method, and no differences were observed among them. MgSO4 and PSA were selected as the final clean-up conditions. We used LC-MS/MS considering the selectivity and sensitivity of the target pesticide and analyzed the samples in the MRM mode. The recovery test results using the established analysis method and inter-laboratory validation showed a valid range of 73.5-100.7%, with a relative standard deviation and coefficient of variation less than 12.6% and 14.5%, respectively. Therefore, the presence of trifludimoxazin can be analyzed using a modified QuEChERS method, which is widely available in Korea to ensure the safety of residual insecticides.

Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.1
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    • pp.22-29
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    • 2019
  • Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural samples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5 ng) into a blank extract with $R^2$ > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respectively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guideline (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determination in agricultural commodities.

Development of a Simultaneous Analytical Method for Determination of Herbicide Fenquinotrione and KIH-3653-M-2 Residues in Agricultural Crops using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 제초제 fenquinotrione 및 대사산물 KIH-3653-M-2 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Cho, Sung Min;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.242-250
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    • 2019
  • An analytical method was developed for the determination of fenquinotrione, a triketone herbicide, in agricultural products. Fenquinotrione was metabolized to KIH-3653-M-2 in plants. Analyte extraction was conducted using 2% formic acid in acetonitrile and cleaned up using a hydrophillic-lipophillic balance (HLB) cartridge. The limits of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. Matrix-matched calibration curves were linear over the calibration ranges ($0.001{\sim}0.1{\mu}g/mL$) into a blank extract with $r^2>0.99$. The recovery results for fenquinotrione and KIH-3653-M-2 ranged between 81.1 to 116.2% and 78.0 to 110.0% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$) with relative standard deviation (RSD) less than 4.6%. All values were corresponded with the criteria ranges requested in both the Codex (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of fenquinotrione in the Republic of Korea.

Residual Characteristics of a Systemic Insecticide Flonicamid and Its Metabolites in Sweet Pepper (착색단고추 중 침투성농약 플로니카미드 및 대사물질의 생성 및 잔류양상)

  • Seo, Eun-Kyung;Kim, Taek-Kyum;Hong, Su-Myeong;Kwon, Hye-Young;Gwon, Ji-Hyeong;Cho, Nam-Jun
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.228-235
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    • 2014
  • The residue levels of flonicamid and its metabolites, 4-(trifluoromethyl)nicotinic acid (TFNA) and N-4-(trifluoromethyl)nicotinoyl glycine (TFNG) in sweer pepper were investigated to examine the residual characteristics of analytes for 87 days after pesticide application. The pesticide was applied once at recommended dosage and double dosage by foliar sprays and the samples of fruits and leaves of sweet pepper were collected for each treatment. The residues of flonicamid in all of fruits and leaves decreased gradually over time, while the residue levels of TFNG metabolite exhibited tendency that increased for long periods and thereafter decreased. Total flonicamid residual concentrations containing metabolites residues in fruit samples increased consistently until 30 days post-application and higher residue levels than residues at 1 day post-application were detected from 30 day to 87 day after treatment. The residue pattern observed in fruit could be explained by the movement of TFNG from leaves to fruits of plant. Such residual characteristic was similarly found in samples treated both recommended dosage and double dosage.