• Title/Summary/Keyword: 잔류용매

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Evaluation of QuEChERS Method for Determination of pesticide Residues Using GC/NPD and GC/ECD (GC/NPD와 GC/ECD를 이용한 잔류농약 정량 분석법으로써의 QuEChERS의 평가)

  • Cho, Tae Hee;Park, Young Hye;Park, Hye Won;Hwang, Lae Hwong;Cho, In Soon;Kim, Min Jung;Kim, Hyun Jeong;Kim, Mu Sang;Chae, Young Zoo
    • The Korean Journal of Pesticide Science
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    • v.17 no.1
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    • pp.65-71
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    • 2013
  • The modified QuEChERS method was evaluated for rapid determination of pesticide residues in spinach by gas chromatography-nitrogen phosphorous detector (NPD) and electron capture detector (ECD). Fifty GC-amenable pesticides which were most frequently detected in monitoring were selected in the current study. Matrix-matched calibration was performed. The detector response for all pesticides was linear with determination coefficients higher than 0.995. LODs for most compounds ranged between 0.001 and 0.1 ug/g, and about 90% of the compounds had LODs of less than 0.05 ug/g. LOQs ranged from 0.001 to 0.32 ug/g, which were well below the MRLs permitted for most of pesticides. In the majority of cases, the recoveries (80-120%) and relative standard deviations (RSDs) (less than 20%) were within acceptable levels except for dichlorvos, propamocarb, chlorothalonil, dichlofluanid, cyhalothrin and fenvalerate. Also, this method which is applied to routine samples showed good results when comparing with traditional multi-residue method.

Determination of Ethylenethiourea in Fruits (과실류에 잔류하는 Ethylenethiourea 분석)

  • Kim, Eun-Hee;Jang, Mi-Ra;Kim, Jin-A;Kim, Tae-Rang;Yook, Dong-Hyun;Hwang, In-Sook;Kim, Jung-Hun
    • Korean Journal of Food Science and Technology
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    • v.43 no.3
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    • pp.277-281
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    • 2011
  • A rapid and very sensitive high-performance liquid chromatography/atmospheric-pressure chemical-ionization mass spectrometry method to detect ethylenethiourea (ETU) fungicide residues in fruits was developed. Methylene chloride was used as the surface extraction solvent for the target component. Recovery rates improved when cysteine hydrochloride and sodium carbonate were added to product prior to fortification. The limits of detection and quantification were approximately 0.006 and 0.02 mg/kg, respectively, from mandarin oranges. Recoveries from mandarin oranges, oranges, bananas, and pears, spiked in the range of 0.05-0.5 mg/kg, averaged 80-100%. The proposed method was used to monitor the presence of ETU in commercial fruits purchased from different markets in Seoul, Korea. ETU was found in four orange peels and in three mandarin orange peel samples. The highest ETU residue levels were $73.6{\mu}g/kg$ and $29.8{\mu}g/kg$.

Residual Pesticide Analysis Method of Edible Oil via Heat Distillation Methods (가열증류법에 의한 식용유지의 잔류농약 분석법 개발)

  • Mi-Hui Son;Jae-Kwan Kim;Young-Seon Cho;Na-Eun Han;Byeong-Tae Kim;Myoung-Ki Park;Yong-Bae Park
    • Journal of Food Hygiene and Safety
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    • v.38 no.3
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    • pp.89-98
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    • 2023
  • Currently, no guidelines exist regarding the maximum residues of pesticides in edible oil which is a processed food commonly consumed in Korea. This lack of guidelines hinders the evaluation of the safety of edible oil in terms of pesticide contamination. In this study, an analysis method based on heat distillation and GC-MS/MS was established by optimizing the extraction and purification procedure for 68 pesticides. Important variables in the thermal distillation procedure included heating temperature and time, and we found the nitrogen flow rate as a mobile phase and the type of dissolving solvent were not considerably affected. The determination coefficient (R2) of the residual pesticide was 0.99 or higher, and the quantitative limit (LOQ) was 0.01-0.02 mg/L. The average recovery rate (n=5) was 66.1-120.0% and the relative standard deviation was lower than ±10% when 68 pesticides were spiked at concentrations of 0.01-0.02, 0.1, and 0.5 mg/L. In addition, the within-laboratory precision was less than ±11%, meeting the Korea Food and Drug Safety Evaluation Institute's Guidelines on Standard Procedures for Preparing Food Testing Methods (2016). Therefore, the test method developed in this study can be used as a test method for managing the safety of the residual pesticide concentration in edible oil.

Heme 촉매반응에 의한 PCP 오염토양 복원

  • ;;D.K.Stevens
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 1996.11a
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    • pp.122-127
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    • 1996
  • 본 실험은 미국 Washington 주 V 도시에서 1987년과 1908년에 PCP 유출사고로 발생된 PCP 오염토양을 처리하는 연구로 heme과 과산화수소를 이용한 abiotic 기술로 14C-PCP를 이용하여 PCP의 거동조사로 물질수지 연구와 pan 연구를 통하여 오염토양에서 PCP 제거되는 분해능을 조사하였다. $^{14}$ C-PCP를 이용한 오염토양에서 물질수지는 2g 오염토양당 0.035 g heme과 0.11g 과산화수소를 첨가하여 반응 24시간 동안 반응시킨후 완전 산화율은 20%, 토양잔류 27%, 그리고 용매상에는 38%로 총 $^{14}$ C-PCP가 회수율은 85% 이었다. PCP 유출사고로 보관된 오염토양 처리를 위한 pan 연구결과 24시간내 초기 PCP 987 mg/kg soil에서 85%가 제거되고, 서서히 분해되어 33일 에는 95% 분해능을 보여주고 있다.

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Acetone-Butanol Fermentation of Rice Straw by Simultaneous Saccharification and Fermentation (동시당화 발효법에 의한 볏짚의 Acetone-Butanol 발효)

  • 권기석;전영숙;김병홍
    • Korean Journal of Microbiology
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    • v.26 no.3
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    • pp.278-282
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    • 1988
  • Rice straw was used in the acetone-butanol fermentation by semultaneous saccharification and fermentation (SSF) using Clostridium acetobutylicum and cellulolytic enzyme. Over 230 mM of solvent was produced from alkali treated rice straw of from ball-milled microcrystalline cellulose whilst only acidic fermentation products were formed from ball-milled rice straw. From the results it is concluded that rice straw used in the study contained an inhibitor for the solventogenesis by the organism which is insoluble in water and some organic solvent and destroyed by alkaline treatment.

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Fabrication of Water-based Ceramic Tapes Using PVP As Binder (PVP 결합제를 이용한 수계용 세라믹테이프의 제조)

  • 박일석;조유정;이명현;최세영;이득용;김대준
    • Journal of the Korean Ceramic Society
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    • v.38 no.11
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    • pp.1060-1066
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    • 2001
  • Water-based alumina tapes for application of all-ceramic crowns were fabricated using PVP as binder that is biocompatible, highly soluble in solvents, and no residue leftafter firing. Tensile strength of alumina tapes was governed by binder/(binder+plasticizer)ratio. On the other hand, linear shrinkage and density were determined by alumina/(alumina+organic) ratio. Composite for all-ceramic crowns, prepared by infiltration of a glass into sintered porous alumina, showed high flexural strength which increased with increasing sintered density.

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Fate of the herbicide bensulfuron-methyl in a soil/rice plant microecosystem (벼 재배 microecosystem 내에서 제초제 bensulfuron-methyl의 행적)

  • Lee, Jae-Koo;Fuhr, F.;Kwon, Jeong-Wook;Ahn, Ki-Chang;Park, Ju-Hyoung;Lee, Yong-Pil
    • The Korean Journal of Pesticide Science
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    • v.8 no.4
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    • pp.299-308
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    • 2004
  • In order to elucidate the behavior of bensulfuron-methyl, a sulfonylurea herbicide, in a soil/plant microecosystem, rice plants (Oryza sativa L.) were grown for 12 weeks in the specially made stainless steel pots (17cm I.D. $\times$ 10cm H.) containing two different paddy soils treated with fresh and 13-week-aged residues of [phenyl-$^{14}C$]bensulfuron-methyl, respectively. During the aging period, the mineralization to $^{14}CO_2$ from soil A (OM, 3.59%; CEC, 7.65 $cmol^+\;kg^{-1}$; texture, sandy clay loam) and B (OM, 1.62%; CEC, 4.51 $cmol^+\;kg^{-1}$; texture, sandy loam) amounted to 6.79 and 10.15% of the originally applied $[^{14}C]$bensulfuron-methyl, respectively. The amounts of $^{14}CO_2$ evolved from the soils with fresh residues were higher than those from the soils with aged residues. At harvest after 12-week growing, $^{14}C$-radioactivity absorbed and translocated into rice plants from soils A and B containing fresh residues of bensulfuron-methyl was 1.53 and 4.40%, while 4.04 and 6.37% in the two soils containing aged residues, respectively. Irrespective of aging and soil type, the $^{14}C$-radioactivity remaining in soil ranged from 80.41 to 98.87% of the originally applied $[^{14}C]$bensulfuron-methyl. The solvent extractability of tile soils was $39.25\sim70.39%$, showing the big differences among the treatments. Most of the nonextractable soil-bound residues of $[^{14}C]$bensulfuron-methyl were incorporated into the fulvic acid fraction$(61.32\sim76.45%)$. Comparing the microbial activity of the soils with rice plants grown with that of the soils without them, the former was $1.6\sim3.0$ times higher than the latter. However, it did not correlate with the $^{14}CO_2$ evolution.

Extraction properties and chemical stability of turmeric pigments in salt, sucrose, and acetic acid preservation (염, 당, 산 침지조건에서 심황색소의 추출특성 및 화학적 특성 변화)

  • Kang, Smee;Sung, Yunkyung;Hong, Jungil
    • Korean Journal of Food Science and Technology
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    • v.52 no.1
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    • pp.19-25
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    • 2020
  • Turmeric pigments have been used as coloring agents and functional ingredients. In this study, the extraction property and chemical stability of the pigments were evaluated in several preservative solutions containing NaCl, sucrose, and acetic acid. After 72 h of infusion, the protein and polyphenol levels and antioxidant activity of the turmeric extracts in the solutions were less pronounced than those in water. Acetic acid (12%) was more efficient at extracting curcuminoids from turmeric than water, NaCl (20%), or sucrose (25%). Curcumin was highly abundant in all solutions. The relative yield of bisdemethoxycurcumin (BMC) was the highest in acetic acid, whereas that of curcumin was highest in NaCl and sucrose solutions. Curcuminoids were relatively stable in sucrose and acetic acid; among them, BMC had the highest stability. The stability of the curcuminoid solution decreased based on the increase in NaCl content, whereas it was significantly enhanced in sucrose and acetic acid. The observations from this study can be applied to the processing and storage of turmeric-derived products in these preservative agents.

Extraction Efficiencies of Organophosphorus Pesticides Spiked in Fish Tissues by Supercritical Carbon Dioxide (초임계 이산화탄소에 의한 어류조직 중 유기인계 농약의 첨가회수율)

  • Lim, Sang-Bin;Jwa, Mi-Kyung
    • Korean Journal of Food Science and Technology
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    • v.30 no.5
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    • pp.1163-1168
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    • 1998
  • Fish tissues were spiked with organophosphorus pesticides (OPPs), mixed with a celite as a drying agent, and dynamically extracted with pure $CO_2$ or modified $CO_2$ for 10 min at different extraction temperatures, pressures and $CO_2$ flow rates. Recoveries of OPPs spiked in jacopever increased with the decrease of extraction temperature and pressure, and decreased with the increase of $CO_2$ flow rates. Modified $CO_2$ extractions with 10% methylene chloride showed a slight increase in the recoveries over pure $CO_2$ extraction. Quantity of fish tissues had great effect on their extraction efficiencies. Recoveries of OPPs were $66.7{\sim}86.3%$ for jacopever, $56.2{\sim}79.2%$ for yellow tail, $57.6{\sim}77.8%$ for blanquillo, $84.2{\sim}96.3%$ for sardine, $74.6{\sim}83.6%$ for mackerel. Application of supercritical carbon dioxide extraction offers an attractive alternative to the use of organic solvents for extraction of pesticide residues from fish tissues.

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Efficiency of Eluting Solvents for Solid-Phase Extraction During Multiresidue Analysis of 16 Pesticides in Cucumber (고상추출카트리지를 이용한 잔류농약 다중분석과정에서 정제용매에 따른 회수율 비교)

  • Tu, Ock-Ju;Kim, Gyung-Sig;Jeong, Eui-Geun;Kim, Jin-Gon;Kim, Myung-Hee;Jung, Bo-Kyung
    • Korean Journal of Environmental Agriculture
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    • v.21 no.2
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    • pp.90-95
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    • 2002
  • A study was carried out to optimize the cleanup step using a solid-phase extraction (SPE) cartridge, $SupelClean^{TM}$ Florisil, for multiresidue analysis of 16 pesticides in cucumber matrix. Eluting efficiencies of two solvent systems including acetone/n-hexane and ethyl acetate/n-hexane mixtures were critically evaluated by recoveries of target anaytes from the SPE Florisil column. Based on the recovery as a measure of eluting efficiency, an acetone/n-hexane (20/80,v/v) mixture provided more than 80% recovery for 15 pesticides except bifenthrin. In case of ethyl acetate/n-hexane, 14 pesticides showed recoveries higher than 75% while those far alachlor and bifenthrin were less than 30%.