• Title/Summary/Keyword: GC-MS (SIM)

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Determination of Polybrominated Biphenyls in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 Polybrominated Biphenyls의 분석법)

  • Hong, Jongki;Baek, In-Girl;Kim, Hyub;Kim, Do-Gyun;Seo, Jung-Joo;Seo, Jong-Bok;Park, Hyun-Mee;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.666-674
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    • 2000
  • The present study describes an analytical method for the determination of polybrominated biphenyls (PBBs) in biota samples by gas chromatography-mass spectrometry (GC/MS). PBBs are extracted twice from 20 g samples with mixture solvent 40mL acetone and 80mL hexane using ultrasonic agitation for 20 min. Lipids in extracts are degraded by concentrated sulfuric acid and then PBBs are purified with Florisil column. The purified extracts are analyzed by GC/MS-selected ion monitoring mode for the quantitation of PBBs in biota sample. The overall recovery yields of PBBs range between 77 and 111% under these experimental conditions.

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Thermal Degradation of High Molecular Components Obtained from Pyrolysis of Mixed Waste Plastics (혼합폐플라스틱의 열분해로부터 생성된 고분자성분의 열적분해)

  • Oh, Sea Cheon;Ryu, Jae Hun;Kwak, Hyun;Bae, Seong-Youl;Lee, Kyong-Hwan
    • Applied Chemistry for Engineering
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    • v.19 no.2
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    • pp.191-198
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    • 2008
  • The thermal degradation characteristics of high molecular components obtained from pyrolysis of mixed waste plastics have been studied by thermogravimetric analysis (TGA) and gas chromatography spectrometry (GC-MS). The kinetics of thermal degradation has been studied by a conventional nonisothermal thermogravimetric technique at several heating rates between 10 and $50^{\circ}C/min$. The dynamic thermogravimetric analysis curve and its derivative have been analyzed using a variety of analytical methods reported in the literature to obtain information on the kinetic parameters such as activation energies and reaction orders. The yields of liquid products have been monitored by batch pyrolysis reactor under various reaction temperatures and reaction times. And the characteristic of liquid products with the increase in reaction temperature has been performed by GC-MS.

Comparative study on some quality-related components of different floral honeys -esp. on the contents of unsaturated higher fatty acids- (벌꿀의 밀원별(蜜源別) 품질관련성분(品質關聯成分)의 비교연구(比較硏究) -불포화(不飽和) 고급지방산(高級脂肪酸)의 함량(含量)에 대하여-)

  • Lee, Young-Gun;Min, Byoung-Uk;Lim, Sun-Uk
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.102-109
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    • 1991
  • Quality of three kinds of honey from acacia, chestnut and polyflower sources, was evaluated by physicochemical and GC-MS analysis in respect to some chemical composition. The average contents of moisture, ash, HMF(hydroxy methyl furfurol) and free acidity were 19.7% , 0.028% , 18.28mg/kg and 8.85meq/kg , respectively, in acacia honey, 19.1% , 0.05% , 18.47mg/kg and 10.24 meq/kg , respectively, in polyflower honey, and 18.9% , 0.050% , 20.21mg/kg, 12.28meq/kg respectively, in chestnut honey. The average contents of glucose and fructose ranged from 31.0 to 32.0% and from 35.0 to 36.0% , respectively, in all three kinds of honey. The average ratio of fructose to glucose was 1.14 in all three kinds of honey. Fatty acid composition in honey identified by GC-MS analysis was dodecanoic acid, 10-hydroxy-2-decanoic acid, 6,9-undecadienoic acid, tetradecanoic acid, 12-(acetyl oxy) -9-octadecenoic acid and 14-octadecenoic acid. The content of 10-hydroxy-2-decenoic acid was about 10% in three kinds of honey.

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The measurement of dicamba in soil and plants (토양 및 식물 중 디캄바 측정법에 대한 연구)

  • Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.480-487
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    • 2009
  • The herbicide dicamba (2-methoxy-3,6-dichlorobenzoic acid) in soil and plants was determined by gas chromatography-mass spectrometry (GC/MS). The samples were extracted with diethyl ether at pH 2, and washed with 0.1 N HCl, and then dried. The dried residue was derivatized in 1 mL of 10% $H_2SO_4$-MeOH for 2 hr at $80^{\circ}C$. The reaction mixture was neutralized with 4 mL of sodium bicarbonate solution and reextracted with 5 mL of diethyl ether. After the extract was concentrated, dicamba was determined by GC/MS-SIM mode. There was good linearity above 0.999 in the ranges of the $1.0{\sim}100{\mu}g/kg$. Total 42 sample including 32 soil samples and 10 plants samples were analyzed by developed method. Dicamba was detected in the concentration range of $2.9-123.9{\mu}g/kg$ in 15 samples among 32 soil samples and in the concentration range of $43-33,252{\mu}g/kg$ in 5 samples among 10 plants samples. A cause of the wither and die of the pine trees is suspected to spray dicamba around or directly to them.

Composition and Antimicrobial Activities of Essential Oils in the Peel of Citrus Fruits

  • Oh, Hyun-Jeong;Ahn, Hyo-Min;Kim, Sang-Suk;Yun, Pil-Yong;Jeon, Gyeong-Lyong;Ko, Young-Hwan;Riu, Key-Zung
    • Journal of Applied Biological Chemistry
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    • v.50 no.3
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    • pp.148-154
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    • 2007
  • Volatile components of the essential oils of Satsuma mandarin (C. unshiu), Dangyuza (C. grandis), Yuza (C. junos), Byungkyul (C. playtymamma), Jinkyul (C. sunki), and Hakyul (C. natsudaidai) grown in Jeju Island were isolated from the fruit peels by hydro distillation and determined by GC-MS. GC-MS analysis identified 58 compounds, with main components being d-limonene $(64.01{\sim}79.34%),\;{\beta}-myrcene\;(3.01{\sim}26.53%),\;{\gamma}-terpinene\;(0.11{\sim}12.88%),\;{\beta}-pinene\;(0.78{\sim}4.74%),\;and\;{\alpha}-pinene\;(1.01{\sim}2.55%)$. Differences in compositions and contents of the essential oils were observed among citrus varieties. Effects of citrus oils on growth inhibitions of Escherchia coli, Staphyllococcus epidermidis, and Candida albicans were investigated using disc diffusion assay and minimal inhibitory concentration (MIC) assay. The essential oils inhibited growths of the test organisms, exhibiting higher levels of activity against Gram-positive S. epidermidis (MIC values $0.04{\sim}0.17mg/mL$), whereas Gram-negative E. coli was moderately resistant (MIC values $1.66{\sim}20.30mg/mL$). MIC of citrus essential oils ranged from $0.82{\sim}23.69mg/mL$ against C. albicans. The essential oils obtained from C. sunki, C. grandis, and C. playtymamma showed the highest antimicrobial activities against S. epidermidis and C. albicans, indicating their potential as natural antimicrobial agents.

Determination of 25 EDs in Frog and Fish Tissue by GC-MS (SIM)

  • Shin, Ueon-Sang;Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.24 no.4
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    • pp.413-420
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    • 2003
  • A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of neutral and bacis twenty-five disruptors $(ED_S)$ in frog and fish. Afther homogenization and sonication of 5 g of sample, purification was achieves in one step with a solid phase extraction procedure using silica gelflorisl. Eluton was performed with 50mL of acetone : n-hexane (1 : 9) solution. The eluate was concentrated to approximately 10uL and dissolves with 100 uL of hexane and analyzed by GC-MS (SIM). The peaks had good chromatographic properties and the extraction of these compounds from sample also gave relatively high recoveries with small variatoins. Detection limits were 0.1 ng/g for 4-nitrotoluene, benzophenone, hexachlorobenzene, atrazine, malathion, o,p-DDT, o,p-DDT and permethrin, and 0.2 ng/g for heptachlor epoxide, γ-chlordane, α-chlordane, p,p'-DDE, p,p'-DDD, cypermethrin and fenvalerate, and 0.3 ng/g for trifluralin, metribuzin, alachlor, dieldrin and p,p'-DDT, and 0.5 ng/g for heptachlor, aldrin and parathion, and 0.7 ng/g for endrin, and 0.8 ng/g for nitrofen. The recoveries were between 33 and 109%. The method was used to analyze twenty-five frogs and forty-six fishes fishes samples caught from various regions in Korea. Benzophenone was detected at concentration of up to 17.2 ng/g in frog or fish. Heptachlor, aldrin, γ-chlordane, p,p'-DDE, p,p'-DDD, endrin and o,p-DDD were detected at concentrations of 0.7-12.5 ng/g in frog or fish. Also significant leveles of dieldrin (up to 22.5 ng/g) were observed. The developed method may be valuable to be used to the national monitoring project of EDS in biota samples.

Simultaneous Determination of Plasticizers in Food Simulants Using GC/MS

  • Park, Na-Young;Yoon, Hae-Jung;Kwak, In-Shin;Jeon, Dae-Hoon;Choi, Hyun-Chul;Eum, Mi-Ok;Kim, Hyung-Il;Sung, Jun-Hyun;Kim, So-Hee;Lee, Young-Ja
    • KOREAN JOURNAL OF PACKAGING SCIENCE & TECHNOLOGY
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    • v.15 no.3
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    • pp.93-98
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    • 2009
  • Migration levels of plasticizers, di-n-butyl phthalate (DBP), benzyl-butyl phthalate (BBP), di-n-octyl phthalate(DNOP), di-iso-decyl phthalate (DIDP) and di-iso-nonyl phthalate (DINP), di-(2-ethylhexyl) adipate (DEHA), from 46 poly(vinyl chloride) (PVC) wrap films and 54 PVC gaskets into food simulants were determined using gas chromatography/mass spectrometry (GC/MS). The method was validated with limit of detection (LOD) of $0.01{\sim}0.02\;{\mu}g/mL$ for DBP, BBP, DNOP and DEHA, and $2\;{\mu}g/mL$ for DIDP and DINP. The linearity were found to be > 0.99 for all the compounds in concentration range of $0.1{\sim}81.4\;{\mu}g/mL$, and overall recoveries were ranged from 90.4 ~ 99.6%. DBP, BBP, DNOP, DEHA, DIDP and DINP were not detected in food simulants, except 1 wrap sample from which 0.28 and $0.99\;{\mu}g/mL$ of DEHA were detected respectively when tested with 20% ethanol and n-heptane as food simulants. These values were below the regulatory limitation in European Union (EU).

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A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구)

  • 이은섭;이용욱
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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Determination of Phthalic Acid Esters and Adipate in Sediment Samples (저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Yoon, Sung-Ho;Cho, Hyun-Woo;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.360-364
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    • 2002
  • The most common 8 phthalic acid esters (PAEs) and adipate in sediment were measured 5 times from 1999 to 2001 at 11 sites of river in Korea. Ultrasonication extraction with dichloromethane was done for extraction of the sediment. After concentration GC/MS-SIM analysis was performed. Three compounds (DEP, DBP and DEHP) among eight phthalic acid esters were detected from the sediment samples, and the other PAEs were not detected in any samples. DEHP (27.3~63.6%) was detected with higher frequency than any other compounds for sediment samples. And this compound had shown the highest average concentration (81.7~427.6 ng/g).

Determination of Phthalate Esters and Adipate in Water and Sediment Samples (수질 및 저질중의 프탈산 에스테르와 아디피산 분석)

  • Myung, Seung-Woon;Chang, Yoon-Jung;Min, Hye-Ki;Kim, Myung-Soo
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.616-623
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    • 2000
  • The most common phthalate acid esters (8 compounds) and adipate were determined from water and sediment simultaneously. After liquid-liquid extraction with n-hexane for water and sonication extraction with dichloromethane for sediment, these were determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.993$) on the range of the 0.1-20 ng/ml (water) and 10-500 ng/g (sediment), and the detection limits of method were below 0.1 ng/ml and 10 ng/g for water samples and sediment samples, respectively. The method shows a good precision and accuracy for measurement of phthalates and adipate.

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