• Title/Summary/Keyword: 크로마토그래피

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Determination of Methoxyfenozide, Chromafenozide and Tebufenozide Residues in Agricultural Commodities Using HPLC-UVD/MS (HPLC-UVD/MS를 이용한 작물 중 methoxyfenozide, chromafenozide 및 tebufenozide의 분석법 확립)

  • Lee, Su-Jin;Kim, Young-Hak;Hwang, Young-Sun;Kwon, Chan-Hyeok;Do, Jeong-A;Im, Moo-Hyeog;Lee, Young-Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.14 no.1
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    • pp.37-48
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    • 2010
  • The diacylhydrazine insecticides, methoxyfenozide, chromafenozide and tebufenozide are new-generation insecticides. These insecticides induce premature molting and cause the death of insects by mimicking their hormone. Also, these insecticides have already been widely used for vegetables planting in worldwide. Highperformance liquid chromatography (HPLC) is the most widely used procedure for determination of each compound residues in crops. However, simultaneous analysis method of these diacylhydrazine insecticides was not reported. The purpose of this study is to develop a simultaneous determination procedure of methoxyfenozide, chromafenozide and tebufenozide residue in crops using HPLC-UVD/MS method. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover these insecticides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were quantitated by HPLCUVD/MS, using a $C_{18}$ column. The crops were fortified with each insecticide at two levels per crop. Mean recoveries ranged from 89.0 to 104.8% in five representative agricultural commodities. The coefficients of variation were less than 3.9%. Quantitative limits of methoxyfenozide, chromafenozide and tebufenozide were 0.04 mg/kg in crop samples. A HPLC-UVD/MS with selected-ion monitoring was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of methoxyfenozide, chromafenozide and tebufenozide in agricultural commodities.

Test Method Using VOC Analyzer to Measure VOC Emission of Paints for Wood-based Panel (VOC Analyzer를 이용한 목재용 도료의 휘발성유기화합물의 간이측정)

  • Eom, Young Geun;Kim, Ki-Wook;An, Jae-Yun;Kim, Hyun-Joong;Moon, Suck-Joong
    • Journal of the Korean Wood Science and Technology
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    • v.35 no.6
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    • pp.65-72
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    • 2007
  • The VOC (volatile organic compound) analyzer is devised to measure the four main aromatic hydrocarbon gases: toluene, ethylbenzene, xylene and styfene. It is not affected by ambient temperature and humidity. In addition, standby and measuring time of VOC Analyzer is a short as below 30 min and 8 min, respectively. Since the semiconductor gas sensor is supersensitive to gas components, it is not necessary to use a conventional gas concentrator or other complicated equipment. In this study, VOC emission behavior from 4 types paints (lacquer, urethane vanish, water-base paint, enamel paint) for wood-based panel was investigated using VOC Analyzer. After a specimen was spreaded on aluminum foil ($6.32{\times}6.32cm$) in $3{\ell}$ polyester bag, after 24 hours we could measure maximum VOC emission level that is a stabilized VOC value. Xylene of VOCs was high emitted from lacquer, urethane vanish and water-based paint, and TVOC (Toluene + Ethylbenzene + Xylene + Styrene) of lacquer was the highest emission concentration than another.

Studies on Biological Activity of Wood Extractives (X VIII) -Isolation and Antioxidant Activity of Chemical Constituents from Maackia amurensis- (수목추출물의 생리활성에 관한 연구(X VIII) -다릅나무(Maackia amurensis) 수피의 추출성분의 분리 및 항산화 활성-)

  • Kim, Woo-Jin;Lee, Hak-Ju;Lee, Sang-Keug;Kang, Ha-Young;Choi, Don-Ha;Choi, Tae-Ho
    • Journal of the Korean Wood Science and Technology
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    • v.35 no.6
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    • pp.135-144
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    • 2007
  • The dried barks of Maackia amurensis were ground, extracted with 95% EtOH, concentrated, and fractionated with a series of light petroleum ether, dichloromethane, ethyl acetate and water on a separatory funnel. Each fraction was concentrated, then a portion of dichloromethane and ethyl acetate soluble was chromatographed on a Sephadex LH-20 and silica gel 60 column using a various solvent system as eluents. The isolated compounds were identified by cellulose TLC, $^1H-$, $^{13}C-NMR$, COSY, NOESY, HMQC, HMBC, FAB and EI-MS. The structures were determined as: 7-O-$\beta$-D-glucopyranosyl-4'-methoxyisoflavone, 7-O-$\beta$-glucopyranosyl(1'''->6'')-$\beta$-D-glucopyranosyl-4'-methoxyisoflavone, 7-O-$\beta$-D-glucopyranosyl(1''''->6''')-$\beta$-D-glucopyranosyl(1'''->6'')-$\beta$-D-glucopyransoyl-4'-methoxyisoflavone, 7-O-$\beta$-D-glucopyranosyl-4', 6-dimethoxyisoflavone. The Free radical scavenging activity using DPPH of the isolated compounds were similar with that of BHT but lower than of $\alpha$-tocopherol.

Novel substrate specificity of a thermostable β-glucosidase from the hyperthermophilic archaeon, Thermococcus pacificus P-4 (초고온 고세균 Thermococcus pacificus P-4로부터 내열성 β-glucosidase의 새로운 기질 특이성)

  • Kim, Yun Jae;Lee, Jae Eun;Lee, Hyun Sook;Kwon, Kae Kyoung;Kang, Sung Gyun;Lee, Jung-Hyun
    • Korean Journal of Microbiology
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    • v.51 no.1
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    • pp.68-74
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    • 2015
  • Based on the genomic analysis of Thermococcus pacificus P-4, we identified a putative GH1 ${\beta}$-glucosidase-encoding gene (Tpa-glu). The gene revealed a 1,464 bp encoding 487 amino acid residues, and the deduced amino acid residues exhibited 77% identity with Pyrococcus furiosus ${\beta}$-glucosidase (accession no. NP_577802). The gene was cloned and expressed in Escherichia coli system. The recombinant protein was purified by metal affinity chromatography and characterized. Tpa-Glu showed optimum activity at pH 7.5 and $75^{\circ}C$, and thermostability with a half life of 6 h at $90^{\circ}C$. Tpa-Glu exhibited hydrolyzing activity against various pNP-glycopyranosides, with kcat/Km values in the order of pNP-${\beta}$-glucopyranoside, pNP-${\beta}$-galactopyranoside, pNP-${\beta}$-mannopyranoside, and pNP-${\beta}$-xylopyranoside. In addition, the enzyme exhibited exo-hydrolyzing activity toward ${\beta}$-1,3-linked polysaccharide (laminarin) and ${\beta}$-1,3- and ${\beta}$-1,4-linked oligosaccharides. This is the first description of an enzyme from hyperthermophilic archaea that displays exo-hydrolyzing activity toward ${\beta}$-1,3-linked polysaccharides and could be applied in combination with ${\beta}$-1,3-endoglucanase for saccharification of laminarin.

Organic Analysis of Charred Residues on the Pottery in the Proto-Three Kingdom from Joong-do Site, Chuncheon (춘천 중도 유적에서 출토된 원삼국시대 토기 탄착물에 대한 화학적 분석)

  • Kang, Soyeong;Jee, Sanghyun;Kim, Yun Ji;Chang, Hong Sun
    • Journal of Conservation Science
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    • v.29 no.4
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    • pp.437-444
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    • 2013
  • We studied for the chemical characterizations of the charred residues obtained from the ancient potteries in the Proto-Three Kingdom period from archaeological sites in Joong-do, Chuncheon. Organic components of the charred residues were extracted and analysed using mass spectrometry and infrared spectroscopy. Lipid profiles from these samples were not identified in gas chromatography-mass spectrometry. Bulk stable isotope analyses of charred residues was used to infer an average values of the foods prepared. The average carbon isotope values (${\delta}^{13}C$) of the residues are $-14.7{\pm}2.8$‰ (ranging from -8.7‰ to -18.4‰, n=9), and nitrogen isotope values (${\delta}^{15}N$) are $6.2{\pm}1.1$‰ (ranging from -4.4‰ to -7.6‰, n=9). This is the first approach to analyse charred residues using stable isotopic method in Korea. Charred food residues on the interior surface of archaeological pottery can provide valuable information about pottery use and dietary habits of its population.

Determination of Gasoline Brands by the Comparison of Infrared Spectra of Polymeric Dispersants (청정분산제의 적외선 분광스펙트럼 비교를 통한 자동차용 휘발유 제조사의 판별)

  • Kim, Myeonghee;Jang, Youngsik;Jung, Chungseop;Lee, Hyunkee
    • Analytical Science and Technology
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    • v.11 no.6
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    • pp.469-473
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    • 1998
  • The gasoline brands can be determined by gas chromatography. However, determining from the differences in chromatograms is sometimes ambiguous because the gasoline composition is becoming similar from refinery to refinery due to stringent regulations for the protection of the atmospheric environment. To determine the gasoline brands of five refineries in Korea, we have obtained and compared IR spectra of polymeric dispersants which are added to gasoline at several hundreds of ppm levels. Since the deposit control additives used by the five refineries in Korea are different from one another, it is possible to determine the gasoline brands by comparing their IR spectra. A strong and broad C-O stretch absorption peak appears at $1,096cm^{-1}$ for the additives used by A, B, and C refineries, which renders an easy differentiation of the additives from those of D and E refineries. The differentiation of all five gasoline brands are possible due to the characteristic vibrations present in each additive.

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Development of Analytical Method for Fipronil Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Fipronil의 잔류 분석법 개발)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.34 no.4
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    • pp.309-317
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    • 2015
  • BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.

Preparation of Pelletized Porous Adsorbent with Pyrolysis Temperature and Its Toluene Gas Adsorption Characteristics (열분해 조건에 따른 펠렛형 다공성 흡착재의 제조 및 톨루엔 가스 흡착 특성)

  • Kim, Do Young;Kim, Yesol;Cho, Seho;Jung, Jin-Young;Kim, Min Il;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.24 no.6
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    • pp.587-592
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    • 2013
  • In this study, we prepared pelletized porous carbon adsorbent (PCA) according to the different pyrolysis temperature using activated carbon and polyvinyl alcohol (PVA) as a binder for the removal of toluene, which is one of the representative volatile organic compounds (VOCs). We investigated physical characteristics of PCA using FE-SEM, BET, TGA and evaluated their adsorption capacity for toluene using GC. It was confirmed that the formability of pellets composed of the activated carbon, PVA and solvent of mass mixing ratio was 1 : 0.2 : 0.8 was the most outstanding. Toluene adsorption capacity was evaluated by measuring the maximum time when more than 99% of toluene adsorbed on the pellet. The specific surface area of the adsorbent pyrolyzed at $300^{\circ}C$ was measured as 4.7 times in $941.9m^2/g$ compared to that of the unpyrolyzed pellet. Micropore volume and toluene adsorption capacity of PCA increased fivefold to be 0.30 cc/g and thirteenfold to be 26 hours compared to that of the unpyrolyzed pellet, respectively. These results were attributed to the change of pore size and specific surface area due to the PVA content and the different pyrolysis temperature.

Volatile Compounds and Antiproliferative Effects of Dendropanax morbifera on HepG2 Cells (황칠나무의 휘발성 화합물 분석 및 HepG2 세포의 증식 억제 효과)

  • Yang, Seun-Ah;Garcia, Coralia V.;Lee, Ji-Won
    • Journal of Life Science
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    • v.27 no.5
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    • pp.561-566
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    • 2017
  • Dendropanax morbifera Lev. is known in Korea for its golden sap and medicinal properties. The many biological activities of the leaf and stem extracts suggest that this tree could be a valuable source of medicinal compounds for the treatment of various ailments such as dermatitis, migraines, dysmenorrhea, muscle pain, and infectious diseases. However, there is little information on the composition and biological activity of the volatile fraction of D. morbifera. Therefore, in this study, the volatile compounds in leaves, stems, and sap of D. morbifera were isolated using solvent and supercritical fluid extraction (SFE), and analyzed by gas chromatography/mass spectrometry to reveal their chemical composition and identify potential compounds of interest. Fifteen compounds were identified in the leaf extracts, whereas 29 and 3 compounds were identified in the stem and sap extracts, respectively. The volatile profiles obtained using solvent and SFE differed. Esters and aromatic hydrocarbons predominated in the solvent extract of leaves and SFE extract of stems, whereas the solvent extract of stems and SFE extract of leaves contained terpenoids. Limonene, ${\alpha}$-pinene, and ${\beta}$-myrcene were identified in the volatile extract of sap, with limonene representing 96.30% of the total peak area. In addition, the antiproliferative effects of the solvent extracts of leaves and stems were evaluated, revealing that these solvent extracts were particularly effective in decreasing the proliferation of HepG2 cells.

Rapid Gas Chromatographic Screening of Alcoholic Beverages for Volatile and Nonvolatile Organic Acids (기체크로마토그래피법에 의한 알코올 음료내 휘발성 및 비휘발성 유기산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Park, Hyung-Kook;Choi, Kyoung-Sook
    • Korean Journal of Food Science and Technology
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    • v.26 no.2
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    • pp.162-166
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    • 1994
  • A rapid gas chromatographic (GC) profiling method for the simultaneous analysis of volatile and nonvolatile organic acids was applied to alcoholic beverages (white wine, red wine, brandy, and beer). It involves the solid-phase extraction of organic acids using Chromosorb P as the sorbent and diethyl ether as the eluent with subsequent triethylamine treatment. The resulting triethylammonium salts of acids were directly converted to volatile tert.-butyldimethylsilyl derivatives, which were analyzed by dual-capillary column GC and GC-mass spectrometry. From the alcoholic beverages studied, more than 29 organic acids were detected. When the simplified retention infer (RI) spectra of organic acids, and the direct comparisor method between alcoholic beverages and a test sample were attempted to identify a test sample, it was quickly recognized to be a red wine with the 998 ppt match quality value.

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