• Title/Summary/Keyword: Solid-phase

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Continuous Wet Oxidation of TCE over Supported Metal Oxide Catalysts (금속산화물 담지촉매상에서 연속 습식 TCE 분해반응)

  • Kim, Moon Hyeon;Choo, Kwang-Ho
    • Korean Chemical Engineering Research
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    • v.43 no.2
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    • pp.206-214
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    • 2005
  • Heterogeneously-catalyzed oxidation of aqueous phase trichloroethylene (TCE) over supported metal oxides has been conducted to establish an approach to eliminate ppm levels of organic compounds in water. A continuous flow reactor system was designed to effect predominant reaction parameters in determining catalytic activity of the catalysts for wet TCE decomposition as a model reaction. 5 wt.% $CoO_x/TiO_2$ catalyst exhibited a transient period in activity vs. on-stream time behavior, suggesting that the surface structure of the $CoO_x$ might be altered with on-stream hours; regardless, it is probable to be the most promising catalyst. Not only could the bare support be inactive for the wet decomposition reaction at $36^{\circ}C$, but no TCE removal also occurred by the process of adsorption on $TiO_2$ surface. The catalytic activity was independent of all particle sizes used, thereby representing no mass transfer limitation in intraparticle diffusion. Very low TCE conversion appeared for $TiO_2$-supported $NiO_x$ and $CrO_x$ catalysts. Wet oxidation performance of supported Cu and Fe catalysts, obtained through an incipient wetness and ion exchange technique, was dependent primarily on the kinds of the metal oxides, in addition to the acidic solid supports and the preparation routes. 5 wt.% $FeO_x/TiO_2$ catalyst gave no activity in the oxidation reaction at $36^{\circ}C$, while 1.2 wt.% Fe-MFI was active for the wet decomposition depending on time on-stream. The noticeable difference in activity of the both catalysts suggests that the Fe oxidation states involved to catalytic redox cycle during the course of reaction play a significant role in catalyzing the wet decomposition as well as in maintaining the time on-stream activity. Based on the results of different $CoO_x$ loadings and reaction temperatures for the decomposition reaction at $36^{\circ}C$ with $CoO_x/TiO_2$, the catalyst possessed an optimal $CoO_x$ amount at which higher reaction temperatures facilitated the catalytic TCE conversion. Small amounts of the active ingredient could be dissolved by acidic leaching but such a process gave no appreciable activity loss of the $CoO_x$ catalyst.

Radioimmunoassay for Determination of Serum Macrophage Migration Inhibitory Factor (혈중 대식세포 유주 저지 인자 측정을 위한 방사면역측정법)

  • Lee, Tae-Sup;Shin, Seok-Hwan;Song, Jee-In;Woo, Kwang-Sun;Chung, Wee-Sup;Choi, Chang-Woon;Lim, Sang-Moo
    • The Korean Journal of Nuclear Medicine
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    • v.38 no.6
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    • pp.532-539
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    • 2004
  • Purpose: There has been a renewal of interest in Macrophage migration inhibitory factor (MIF), especially correlation in pathogenesis of sepsis by many infectious diseases and in regulation of host inflammatory and immune response. We developed immunoradiometric assay (IRMA) to determine serum human MIF concentration. Materials and Methods: The IRMA system utilizes solid phase bound monoclonal anti-recombinant human MIF (rhMIF) antibody as a capture antibody, biotinylated polyclonal anti-rhMIF antibody as a detector antibody. We applied with rhMIF that concentration of standard solutions increased from 0 ng/ml to 100 ng/ml. We used $^{125}I$-streptavidin (SA) as radiotracer to determination of rhMIF concentration. Streptavidin was labeled with $^{125}I$ by Chloramine-T method and $^{125}I$-SA was purified by ultracentrifugation. $^{125}I$-SA stability was evaluated by ITLC analysis at $4^{\circ}C$ and room temperatures until 60days. To validate IRMA system for MIF, we experimented intra-assay and inter-assay coefficients of variation, recovery test and dilution test. Results: Radiolabeling yield of $^{125}I$-SA was 87% and purified $^{125}I$-SA retained above 99% radiochemical purity. $^{125}I$-SA showed above 93% stability in $4^{\circ}C$ until 60days that it is good for immunoradiometric assay as radiotracer. Plotted standard dose response curve showed that increased concentration of rhMIF linearly correlated (R2=0.99) with bound radioactivity of $^{125}I$-SA. The highest intra- and inter-assay coefficients of variation were 5.5% and 7.6%, respectively. The average of recovery of MIF in samples was 102%. In dilution test, linear response curves were obtained (R2=0.97). Conclusion: Radioimmunoassay using $^{125}I$-SA as radiotracer thought to be useful for the determination of serum MIF concentration, and further, its data will be used to evaluate the correlation between clinical significance and serum MIF concentration in patients with various inflammatory diseases.

Comparison of Fragrance and Chemical Composition of Essential Oils in Gom-chewi (Ligularia fischeri) and Handaeri Gom-chewi (Ligularia fischeri var. spicifoprmis) (곰취(Ligularia fischeri)와 한대리곰취(Ligularia fischeri var. spicifoprmis) 정유의 향취 및 향기성분 비교)

  • Yeon, Bo-Ram;Cho, Hae Me;Yun, Mi Sun;Jhoo, Jin-Woo;Jung, Ji Wook;Park, Yu Hwa;Kim, Songmun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.12
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    • pp.1758-1763
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    • 2012
  • This study was conducted to compare fragrance and volatile chemicals of essential oils in Gom-chewi (Ligularia fischeri) and Handaeri Gom-chewi (Ligularia fischeri var. spicifoprmis). Essential oils were extracted by steam distillation of leaves of Gom-chewi (GC) and Handaeri Gom-chewi (HGC), after which samples were collected by solid-phase micro extraction and the compositions of the essential oils were analyzed by gas chromatography-mass spectrometry (GC-MS). The yields of the essential oils in GC and HGC were 0.12% and 0.04%, respectively, and the threshold levels of the essential oils in GC and HGC were 0.01% and 0.1%, respectively. There were 19 constituents of the essential oil of Gom-chewi: 14 carbohydrates, 4 alcohols, and 1 acetate, and the major constituents were L-${\beta}$-pinene (36.02%), D-limonene (25.64%), ${\alpha}$-pinene (24.85%) and ${\beta}$-phellandrene (5.39%). In the essential oil of HGC, 25 constituents were identified: 17 carbohydrates, 4 alcohols, 3 acetates, and 1 N-containing compound, and the major constituents of HGC were D-limonene (39.74%), L-${\beta}$-pinene (35.43%) and ${\alpha}$-pinene (11.94%). The minor constituents of HGC were ${\rho}$-cymene, ${\gamma}$-muurolene, ${\gamma}$-cadinene, germacrene D, ingol 12-acetate and butyl 9,12,15-octadecatriene and nimorazole were not identified in the GC essential oil. Overall, the results showed that the fragrance and chemical compositions of essential oils in GC and HGC differed, suggesting that both essential oils could be used for the development of perfumery products.

Development of n Hydroponic Technique for Fruit Vegetables Using Synthetic Fiber Medium (합성섬유 배지를 이용한 과채류 수경재배 기술 개발)

  • Hwang Yeon-Hyeon;Yoon Hae-Suk;An Chul-Geon;Hwang Hae-Jun;Rho Chi-Woong;Jeong Byoung-Ryong
    • Journal of Bio-Environment Control
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    • v.14 no.2
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    • pp.106-113
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    • 2005
  • This study was carried out to develop a novel hydroponic medium far fruit vegetable crops by using waste synthetic fibers. In physical analysis of the synthetic fiber medium (SFM), the bulk density and percent solid phase were lower, while the porosity and water content were greater in comparison with the rockwool slab. The SFM had pH of 6.5 and EC of $0.03dS{\cdot}m^{-1}$ both of which are similar to those of the rockwool slab. The CEC of 0.39me/100mL of the SFM was lower than compared with 3.29me/100mL of the rockwool slab. However, concentrations K, Ca, Mg and Na were slightly higher in the SFM than those in the rockwool slab. The 'Momotaro' tomato crop in the SFM gave comparable plant height, stem diameter, days to first flowering, fruit weight and percent marketable yield as the rockwool slab. In the SFM and in the rockwool slab, mean fiuit weight were 182g and 181g, percent marketable yield were $93.8\%$ and $92.0\%$, respectively. The marketable yield per 10a in the SFM was 12,799 kg, which was $97\%$ of that in the rockwool slab. Growth parameters such as leaf length and width, leaf number, stem diameter and chlorophyll content of an exportable cucumber crop grown in the SFM and the rockwool slab were not different. Fruit weight was greater in the rockwool slab, while percent marketable yield was greater in the SFM. The marketable fruit yield per 10a of 5,062kg in the SFM was $2\%$ greater than that in the rockwool slab. $NO_3$ concentration in nutrient solution during the crop cultivation was higher in the SFM than in the rockwool slab, while concentrations $NH_4$, K, Ca, Mg and $SO_4$ were not different between the two media.

Trace Metal Contamination and Solid Phase Partitioning of Metals in National Roadside Sediments Within the Watershed of Hoidong Reservoir in Pusan City (부산시 회동저수지 집수분지 내 국도도로변 퇴적물의 미량원소 오염 및 존재형태)

  • Lee Pyeong-Koo;Kang Min-Joo;Youm Seung-Jun;Lee In-Gyeong;Park Sung-Won;Lee Wook-Jong
    • Journal of Soil and Groundwater Environment
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    • v.11 no.5
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    • pp.20-34
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    • 2006
  • This study was undertaken to assess the anthropogenic impact on trace metal concentrations (Zn, Cu, Pb, Cr, Ni, and Cd) of roadside sediments (N = 70) from No.7 national road within the watershed of Hoidong Reservoir in Pusan City and to estimate the potential mobility of selected metals using sequential extraction. We generally found high concentrations of metals, especially Zn, Cu and Pb, affected by anthropogenic inputs. Compared to the trace metal concentrations of uncontaminated stream sediments, arithmetic mean concentrations of roadside sediments were about 7 times higher for Cu, 4 times higher for Zn, 3 times higher for Pb and Cr and, 2 times higher for Ni and As. Speciation data on the basis of sequential extraction indicate that most of the trace metals considered do not occur in significant quantities in the exchangeable fraction, except for Cd and Ni whose exchangeable fractions are appreciable (average 29.3 and 25.8%, respectively). Other metals such as Zn (51.4%) and Pb (45.2%) are preferentially bound to the reducible fraction, and therefore they can be potentially released by a pH decrease and/or redox change. Copper is mainly found in the organic fraction, while Cd is highest in the exchangeable fraction, and Cr and Ni in the residual fraction. Considering the proportion of metals bound to the exchangeable and carbonate fractions, the comparative mobility of metals probably decreases in the order of Cd>Ni>Pb>Zn>Cr>Cu. Although the total concentration data showed that Zn was typically present in potentially harmful concentration levels, the data on metal partitioning indicated that Cd, Ni and Pb pose the highest potential hazard for runoff water. As potential changes of redox state and pH may remobilize the metals bound to carbonates, amorphous oxides, and/or organic matter, and may release and flush them through drain networks into the watershed of Hoidong Reservoir, careful monitoring of environmental conditions appears to be very important.

Immunogenicity of Synthetic Peptide Specific for Major Immunogenic Determinat of Hepatitis B Surface Antigen (B형간염(型肝炎) 표면항원(表面抗原)의 주면역원(主免疫原) 결정기(決定基)에 특이(特異)한 합성(合成) Peptide의 면역원성(免疫原性)에 관한 연구(硏究))

  • Shin, Kwang-soon;Han, Su-nam
    • Korean Journal of Veterinary Research
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    • v.25 no.1
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    • pp.7-17
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    • 1985
  • Many investigators have been pursuing various attempts so far to produce hepatitis B surface antigen(HBsAg) vaccines using the techniques such as isolation from plasma of chronic HBsAg carrier, recombinant DNA technique or preparation of synthetic peptides specific for immunogenic determinants. Hepatitis B virus can not grow on any cell lines by the tissue culture technique at the present time. The plasma of chronic HBsAg carrier is expensive and its source is limited. The HBsAg from the recombinant DNA technique gave still very low yield. Another approach, therefore, has been initiated to develop a synthetic hepatitis B virus vaccine. The possible use of several distinct synthetic vaccines in prophylaxis can be facilitated by availability of full synthetic immunogens. Peptides synthesized for potential application as antiviral vaccines have been mostly tested in the form of conjugates with carrier proteins, although the free synthetic peptide can be immunogenic. To understand basic knowledges on the antigenicity and immunogenicity of a synthetic peptide specific for major immunogenic determinant of HBsAg, a nonapeptide, $H_2N^{139}Cys-Thr-Lys-Pro-Thr-Asp-Gly-^{146}Asn-Aba$ COOH, which corresponds to HBsAg amino acid residues 139 to 147, was synthesized by the Merrifield's solid-phase method with a slight modification. The antigenicity and immunogenicity of this specific synthetic peptide were examined comparing with purified plasma-derived natural HBsAg. The results obtained are as follows; 1. The peptide synthesized showed the identical amino acid composition to the theoretical value. The degree of purification and molecular weight were acertained by methods of high performance liquid chromatography and mass spectrometry. 2. Using m-maleimidobenzoyl-N-hydroxysuccinimide ester as a conjugating agent, the synthetic peptide was conjugated to rabbit albumin and ${\gamma}$-globulin, tetanus and diphtheria toxoids, and keyhole limpet hemocyanin. Their conjugation yields were 8.3, 9.5, 15.8, 13.5, and 11.2%, respectively. 3. The natural HBsAg was purified from plasma of chronic HBsAg carrier. By the electron microscopic observation of the purified natural HBsAg preparation, no Dane particles were observed and the preparation showed negative DNA polymerase activity. 4. Antigenicity of the synthetic peptide and the plasma-derived natural HBsAg was determined by competition radioimmunoassay using $^{125}I$-natural HBsAg. Their 50% inhibitions appeared as $90{\mu}g/ml$ and $0.12{\mu}g/ml$ for the synthetic peptide and the natural HBsAg, respectively. This indicates that the former was about 750-fold less antigenic than the latter. 5. Immunogenicity of the synthetic peptide was determined by administering the peptide-carrier conjugates into rabbits with and without Freund's complete adjuvant. Regardless the carrier proteins and adjuvant, positive immune responses to the synthetic peptide were observed. The higher antibody titers, however, were shown in the groups administered with Freund's complete adjuvant. 6. Immunizing dose 50% in mice of the various peptide-carrier conjugates was 5.47, 6.00, 65.16, 31.25 and $13.03{\mu}g/dose$ for rabbit albumin and ${\gamma}$-globulin, tetanus and diphtheria toxoids, and keyhole limpet hemocyanin, respectively, while the natural HBsAg showed $0.65{\mu}g/dose$. 7. It was postulated that homologous proteins prefer to heterologous ones as the carriers.

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Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

Identification of Fatty Acids in the Pulp Oils of Jujube and Their Compsitional Changes in the Ripening Period (대추의 과육지질(果肉脂質)에 존재(存在)하는 지방산(脂肪酸)의 동정(同定)과 숙성(熟成)에 따른 그 조성(組成)의 변화(變化))

  • Woo, Hyo-Kyeng;Kim, Seong-Jin;Park, Sung-Hea;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.18 no.1
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    • pp.67-77
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    • 2001
  • In search for several fatty acid with unusual structure in vegetable oils, we have found that unknown peaks were shown on GLC in the analysis of fatty acids of the lipids from the pulp of ripened jujube (Zizypus jujuba var. inermis) fruits. These fatty acids were identified as a series of cis-monoenoic acids with ${\omega}-5$ double bond system such as $C_{14:1{\omega}5}$, $C_{16:1{\omega}5}$ and $C_{18:1{\omega}5}$, including ${\omega}-7$ fatty acid as $C_{16:1{\omega}7}$ and $C_{18:1{\omega}7}$, by GLC, solid-phase extraction silver ion-column chromatographic, GLC-mass spectrometric and IR techniques. First of all, total fatty acid methyl esters were resolved into saturated and branched fatty acid, monoenoic acid, dienoic acid, and trienoic acid fraction, respectively, with 100% dichloromethane (DCM), DCM/acetone (9:1, v/v) 100% acetone, and acetone/ acetonitrile (97:3, v/v) solvent system. Unknown fatty acids were included in the monoenoic fraction and were confirmed to have cis-configuration by IR. Picolinyl esters of monoenoic fatty acids gave distinct molecular ion peak and dominant diagnostic peaks, for example, m/z 317, 220 and 260 fragment for $cis-C_{14:1{\omega}5}$, m/z 345, m/z 248 and 288 fragment for $cis-C_{16:1{\omega}5}$ and m/z 373, m/z 276 and 316 fragment for $cis-C_{18:1{\omega}5}$. In this way the occurrence of $cis-C_{16:1{\omega}7}$ and $cis-C_{18:1{\omega}7}$ could be deduced from the appearance of prominent fragments as m/z 345, 220 and 260, and m/z 373, 248 and 280. Level of total ${\omega}-5$ fatty acids amounted to about 30% in the fatty acid composition with the predominance of $C_{16:1{\omega}5}$ $ (18.7{\sim}25.0%)$, in the semi-ripened and/or ripened samples collected in September 14 ($C_{16:1{\omega}5}$ ; 18.7%, $C_{14:1{\omega}5}$ ; 3.6% and $C_{18:1{\omega}5}$ ; 3.0%), September 22 ($C_{16:1{\omega}5}$ ; 25.0%, $C_{14:1{\omega}5}$ ; 1.4% and $C_{18:1{\omega}5}$ ; 2.6%), and October $7 (C_{16:1{\omega}5}$ ; 24.7%, $C_{14:1{\omega}5}$ ; 7.7% and $C_{18:1{\omega}5}$ ; 2.5%). However, the lipids extracted from unripened jujube in July and August contain these unusual fatty acids as low as negligible. It could be observed that the level of ${\omega}-5$ fatty acids in the pulps increased sharply with an elapse of ripening time of jujube fruits. Other monoenoic fatty acids with ${\omega}-7$ series, $C_{16:1{\omega}7}$ (palmitoleic acid) and $C_{18:1{\omega}7}$ (cis-vaccenic acid) could be detected. And in the lipids of the kernel and leaf of jujube, none of ${\omega}-5$ fatty acids could be detected.

Improvement of Radiosynthesis Yield of [11C]acetate ([11C]아세트산의 방사화학적 수율 증가를 위한 연구)

  • Park, Jun Young;Son, Jeongmin
    • The Korean Journal of Nuclear Medicine Technology
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    • v.22 no.2
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    • pp.74-78
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    • 2018
  • Purpose $[^{11}C]$acetate has been proved useful in detecting the myocardial oxygen metabolism and various malignancies including prostate cancer, hepatocellular carcinoma, renal cell carcinoma and brain tumors. The purpose of study was to improve the radiosynthesis yield of $[^{11}C]$acetate on a automated radiosynthesis module. Materials and Methods $[^{11}C]$acetate was prepared by carboxylation of grignard reagent, methylmagnesium chloride, with $[^{11}C]$$CO_2$ gas, followed by hydrolysis with 1 mM acetic acid and purification using solid phase extraction cartridges. The effect of the reaction temperature ($0^{\circ}C$, $10^{\circ}C$, $-55^{\circ}C$) and cyclotron beam time (10 min, 15 min, 20 min, 25 min) on the radiosynthesis yield were investigated in the $[^{11}C]$acetate labeling reaction. Results The maximum radiosynthesis yield was obtained at $-10^{\circ}C$ of reaction temperature. The radioactivities of $[^{11}C]$acetate acquired at $-10^{\circ}C$ reaction temperature was 2.4 times higher than those of $[^{11}C]$acetate acquired at $-55^{\circ}C$. Radiosynthesis yield of $[^{11}C]$acetate increased with increasing cyclotron beam time. Conclusion This study shows that radiosynthesis yield of $[^{11}C]$acetate highly dependent on reaction temperature. The best radiosynthesis yield was obtained in reaction of grignard reagent with $[^{11}C]$$CO_2$ at $-10^{\circ}C$. This radiolabeling conditions will be ideal for routine clinical application.

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.