• Title/Summary/Keyword: 잔류분석

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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.

Good Agricultural Practices (GAP) analysis of hazardous materials in button mushroom (Agaricus bisporus) (GAP 양송이버섯 재배를 위한 위해물질 분석)

  • Lee, Byung-Eui;Kim, Tae-Hyun;Lee, Chan-Jung;Kim, Yong-Gyun;Lee, Byung-Joo
    • Journal of Mushroom
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    • v.15 no.4
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    • pp.178-182
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    • 2017
  • Good Agricultural Practices (GAP) is the world's leading quality certification for food safety. Since its introduction in Korea in 2006, its importance has been increasing every year. In particular, food safety issues are becoming increasingly important in society, and food safety is directly linked to health. The core of GAP certification is the traceability of the production, distribution, and consumption of hazardous materials, including pesticide residues, heavy metals, and microbes. In the present study, pesticides and heavy metals in button mushroom (Agaricus bisporus) and associated cultivation materials were analyzed. Tricyclozole (0.0144 ppm), flubendiamide (0.147 ppm), and trifloxystrobin (0.0340 ppm) were detected in rice straw and wheat straw, and carbendazim (0.0142 ppm) was detected in mixed wheat straw and rice straw medium. Lead and cadmium were detected at levels higher than the standard level in rice straw and mixed medium. However, lead and cadmium were not detected in mushrooms, and levels of arsenic and mercury were below the safety limit. Therefore, it was confirmed that the residual pesticides and heavy metals are safely managed in the investigated mushroom species. The results of the present study suggest that if these materials are adequately managed in the surroundings during cultivation, all hazardous materials can be managed during mushroom production.

Monitoring of Pesticide Residues and Risk Assessment for Fruits in Market (국내 유통 과실류의 잔류농약 모니터링 및 위해성 평가)

  • Ahn, Ji-Woon;Jeon, Young-Hwan;Hwang, Jeong-In;Kim, Jeong-Min;Seok, Da-Rong;Lee, Eun-Hyang;Lee, Seong-Eun;Chung, Duck-Hwa;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.32 no.2
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    • pp.142-147
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    • 2013
  • BACKGROUND: This study was conducted to monitor residual pesticides in domestic agricultural products and to assess their risk to human health. METHODS AND RESULTS: 123 samples containing both general and environment-friendly certified agricultural products were purchased from traditional domestic markets and supermarkets in six provinces of Korea. Multiresidue analyses of one hundred twenty-two pesticides except for herbicides were performed with gas chromatography-electron capture detector, gas chromatography-nitrogen/phosphorus detector, and high-performance liquid chromatography. Sixteen pesticides were detected in 45 agricultural product samples, which were 38 general, 6 low pesticide and 1 of GAP agricultural product samples and the detection rate was 33.6%. Pesticides detected in agricultural product samples were cypermethrin, lufenuron, fenvalerate, bifenthrin, chlorfenapyr and iprodione. Residual concentration of 18 samples were exceeded the recommended maximum residue limit set by Ministry of Food and Drug Safety and two kinds of unregistered pesticides in korea were also detected in two samples. CONCLUSION(S): In order to do risk assessment by agricultural products 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 0.038% to 2.748%. Taken together, it demonstrates the pesticides found in agricultural products samples were below the safety margin, indicating no effect on human health.

Establishment of the Korean total diet study (TDS) model in consideration to pesticide intake (한국형 총식이섭취조사(Total Diet Study, TDS) 모델 확립을 위한 농약섭취수준에 대한 접근)

  • Yang, An-Gel;Shim, Ki-Hoon;Choi, Ok-Ja;Park, Jong-Hyouk;Do, Jung-Ah;Oh, Jae-Ho;Hwang, In Gyun;Shim, Jae-Han
    • The Korean Journal of Pesticide Science
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    • v.16 no.2
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    • pp.151-162
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    • 2012
  • This study was carried out to establish Korean total diet study (TDS) model for estimating pesticide residue in food samples. In addition, pesticide residues of food samples were monitored by setting the standards of established Korean total diet study model. For monitoring, first step were selection of total 102 species food samples, second step were selection of total 70 species food samples, and third step were selection of total 12 representative diet and 109 species food samples. Ninety-eight pesticides were analyzed using $GC-{\mu}ECD$, GC-MS, and LC-MS/MS after QuEChERS sample preparation method. The residue levels in detected food samples were below the maximum residue limit (MRL). Establishment of the Korean total diet study model means providing safe food for consumers, secure the safety of food samples and provide ongoing information to agricultural producers about use of pesticides.

A Study on Characteristics of Residue in Liquefied Petroleum Gas using Automotive Fuel (자동차용 액화석유가스(LPG) 잔류물질의 특성 연구)

  • Jang, Yoon-mi;Park, Tae-seong;Kang, Hyung-kyu;Yim, Eui Soon;Lee, Jung-min;Na, Byung-gi
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.3
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    • pp.816-825
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    • 2018
  • Recently, it was emerged to need the necessity of LPG residues management due to the finding some substances such as rust. This study is performed to investigate the characteristics of LPG residues in the production and distribution stage of LPG. For the qualitative analysis of LPG residues, it was operated to be set up the analysis conditions(the flow rate, etc) of GC-MS and was performed to analyze the component of LPG residues. From the analysis result using GC-MS, it was shown that the component of LPG residues was turned out the plasticizer to be used in the rubber manufacturing process. The inorganic components of LPG residues were analyzed using ICP-OES. At the results of inorganic analysis, it was shown that the Si element was detected, which was presumably derived from defoamers used mainly in the LPG production. Also, the P and Zn element, which are estimated to be components of grease additives used for filling facilities, were also partially detected. No trace of rusting was detected in the LPG residues in the production and distribution stages analyzed in this study. But, as plasticizers and grease additives can affect to the LPG fuel system in vehicles, it will be necessary to use the proper quality of rubber and to expand the use of low boiling grease additives.

Effect of Normal Operating Condition Analysis Method for Weld Residual Stress of CRDM Nozzle in Reactor Pressure Vessel (원전 정상가동조건 적용 방식이 원자로 압력용기 상부헤드 관통 노즐의 용접 잔류응력에 미치는 영향)

  • Nam, Hyun Suk;Bae, Hong Yeol;Oh, Chang Young;Kim, Ji Soo;Kim, Yun Jae
    • Transactions of the Korean Society of Mechanical Engineers A
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    • v.37 no.9
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    • pp.1159-1168
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    • 2013
  • In pressurized water nuclear reactors (PWRs), the reactor pressure vessel (RPV) upper head contains penetration nozzles that use a control rod drive mechanism (CRDM). The penetration nozzle uses J-groove weld geometry. Recently, the occurrence of cracking in alloy 600 CRDM penetration nozzle has increased. This is attributable to primary water stress corrosion cracking (PWSCC). PWSCC is known to be susceptible to the welding residual stress and operational stress. Generally, the tensile residual stress is the main factor contributing to crack growth. Therefore, this study investigates the effect on weld residual stress through different analysis methods for normal operating conditions using finite element analysis. In addition, this study also considers the effect of repeated normal operating condition cycles on the weld residual stress. Based on the analysis result, this paper presents a normal operating condition analysis method.

Analysis of a Bi-directional Load Test Result on tong PHC Piles in Consideration of Residual Load (잔류하중을 고려한 장대 PHC 말뚝의 양방향 재하시험 결과해석)

  • Kim, Sung-Ryul;Chung, Sung-Gyo;Lee, Bong-Yeol
    • Journal of the Korean Geotechnical Society
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    • v.24 no.6
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    • pp.85-93
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    • 2008
  • For long piles driven in deep clay deposits, it is difficult to estimate the ultimate bearing capacity due to large resistance induced by long embedded depth, and also the load transfer curve due to large residual load induced by negative skin friction, even with the performance of pile load tests. In this research, a hi-directional load test on a PHC pile driven in deep soft deposit was performed in order to evaluate the tip and shaft resistances separately, which are feasible to estimate the ultimate bearing capacity of the pile. Residual load of the pile was determined by continuous monitoring of pile strains after the pile installation. The true resistance and true load-movement curve of the pile were properly estimated by taking account of the residual load. A model far behavior of the shaft resistance vs. movement was also proposed, which includes the effects of residual load based on the experiment. Consequently, it was proved that the residual load should be taken into consideration for correctly analyzing load test results of piles in deep clay deposits.

HPLC를 이용한 우유 중에 잔류 항생물질(Streptomycin)의 정량 분석

  • Byeon, Jang-Won;Park, Hwan-Seok;Hong, Go-Eun;Hong, Mu-Gi;Park, Gwan-Ha;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.310-316
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    • 2005
  • 축산식품(우유)내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/dihydrostreptomycin, neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 STP에 대한 HPLC법에 대한 보고한 Edder 방법 중에 clean-up 과정 및 이동상 조건을 대폭 수정하여 STP의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering La-boratories, Inc.)의 컬럼 온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, 유도체화 용매 유속 0.6ml/min 이동상 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 STP 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 STP의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection(LOD)은 0.02ppm이었으며, 적어도 우유에서의 MRL이 0.6ppm임을 감안하면 STP를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 우유에 표준 STP를 0.5ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 STP의 limit of quantification(LOQ)는 약 0.44ppm이었으며, 이에 대한 회수율은 89.7${\pm}$2.3%(n=6)를 나타냈다. 실제 CODEX에서 권장한 우유의 MRL이 0.6ppm인 점을 감안하면 CODEX권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발 된 시험법은 지금까지 국내적으로 STP에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 STP에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 STP에 대한 분석시험법을 개발하였다.

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Catalytic Pyrolysis of Waste Paper Cup Containing Coffee Residuals (커피 잔류물을 함유한 폐종이컵의 촉매 열분해)

  • Shin, Dongik;Jeong, Seokmin;Kim, Young-Min;Lee, Hyung Won;Park, Young-Kwon
    • Applied Chemistry for Engineering
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    • v.29 no.2
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    • pp.248-251
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    • 2018
  • Catalytic pyrolysis of the waste paper cup containing coffee residual (WPCCCR) was performed using a fixed bed reactor and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS). Non-catalytic pyrolysis of WPCCCR produced a large amount of oil together with gas and char. The use of both HZSM-5 and HY decreased the yields of oil and increased the yield of gas due to the additional catalytic cracking. Owing to the acidic catalytic properties of HZSM-5 and HY, catalytic Py-GC/MS analysis of WPCCCR increased the selectivity to aromatic hydrocarbons in product oil. Owing to properties of HZSM-5 having a stronger acidity and medium pore size, the catalytic pyrolysis of WPCCR over HZSM-5 produced much larger amounts of aromatic hydrocarbons than that of using HY.

Dietary Risk Assessment for Pesticide Residues of Vegetables in Seoul, Korea (서울지역 유통 채소류 섭취에 따른 잔류 농약의 위해성 평가)

  • Jang, Mi-Ra;Moon, Hyun-Kyung;Kim, Tae-Rang;Yuk, Dong-Hyun;Kim, Jung-Hun;Park, Seog-Gee
    • Journal of Nutrition and Health
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    • v.43 no.4
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    • pp.404-412
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    • 2010
  • This paper specifically discusses the risk assessment on the pesticide residues in vegetables collected from traditional markets, big marts and departments in the southern part of Seoul. Vegetable samples were 6,583 cases from January to December in 2009. Monte-Carlo simulation was used to calculate the uncertainty for the risk index using pesticide residues, average dietary intake for vegetables and acceptable daily intake. Deterministic risk indexes were 7.33% of diethofencarb, 5.13% of indoxacarb, 3.96% of EPN, 3.92% of diniconazole and 3.09% of chlorothalonil, respectively. And other pesticides were below 3%. Distributions of risk indexes obtained by the Monte-Carlo simulations were similar to the deterministic values, even though the confidence intervals for 95% were very wide. We confirmed that health risks caused by eating vegetables exceeded maximum residue limits of pesticide are very low and the population is generally safe, judging from the risk indexes located between 0.07 to 9.49%.