• Title/Summary/Keyword: GC and GC-MS method

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Analysis of 12 chlorophenols in waste-water using automated liquid phase microextracion (LPME) device (자동화된 Liquid Phase Microextraction(LPME)를 이용한 폐수 중 12종의 클로로페놀 분석)

  • Kim, Seok-Jung;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.20 no.1
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    • pp.70-77
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    • 2007
  • Twelve chlorophenols (CPs) were extracted by liquid phase microextraction (LPME) from the industrial waste-water and analyzed by GC/MS. To establish the optimal conditions, species of extraction solvent, sample amount, pH of sample, salting out effect, a number of sampling and plunger movement speed were investigated. As a result, the linearities of calibaration curves ranged from 0.9913 to 0.9999, while LODs and LOQs were from 0.05 to 10.0 ng/mL except 2,3,4,5-tetrachlorophenol and pentachlorophenol. Using this method, 4-chloro-3-methylphenol confirmed from waste water at the concentration of 784 ng/mL. The method can be applicable to detect chlorophenols from industrial waste-water.

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1497-1504
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    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon,Chul-Ho;Choi, Choi,Sang-Ki;Kim, Kim,Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.97-97
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

Determination of Polychlorinated Biphenyls in the Soil by Perchlorination (염소화법에 의한 토양 중 Polychlorinated Biphenyls의 잔유분석)

  • Moon, Moon, Chul-Ho;Choi, Choi, Sang-Ki;Kim, Kim, Jung-Ho
    • Journal of Environmental Science International
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    • v.4 no.3
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    • pp.249-258
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    • 1995
  • PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

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Rapid Analytical Method of Volatile- and Semivolatile Organic Compounds in Water and their Monitoring in Water Treatment Plants (물 시료 중 휘발성 및 반휘발성 유기물질들의 빠른 분석법 및 정수처리 단계별 모니터링)

  • Shin, Ho-Sang;Ahn, Hye-Sil
    • Analytical Science and Technology
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    • v.17 no.3
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    • pp.240-250
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    • 2004
  • A gas chromatography-mass spectrometric (GC-MS) assay method was developed for the rapid and sensitive determination of volatile- and semivolatile organic compounds in water. Two hundreds mL of water sample was extracted in a 250 mL separatory funnel with 1 ml of pentane at pH 6.5. Fluorobenzene and 1,2-dichlorobenzene-d4 as internal standards were added to water sample and the solution was mechanically shaken for 5 min and analyzed by GC-MS (selected ion monitoring) without more any concentration or purification steps. The peaks had good chromatographic properties and the extraction of these compounds from water also gave relatively high recoveries with small variations. The range of detection limits of the assay was 0.5-10 ng/L. Turnaround time for up to about 40 samples was one day. This method is simple, convenient, and can be learned easily by relatively inexperienced personnel. This method was used to analyze 15 volatile- and semivolatile organic compounds in water of a Lake, and raw and treated water from three Water Treatment Plants in Korea. As the analytical results, benzene, toluene, xylene, isopropylbenzene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene, naphthalene and 2,4,6-trichlorophenol were detected at concentrations of up to 0.4, 1.9, 1.3, 0.2, 1.8, 13.0, 1.7 and $1.1{\mu}g/L$, respectively. But chlorobenzene, trichloroethylene, tetrachloroethylene, ethylbenzene, n-butylbenzene and dibromochloropropane levels during that period were not significant. The removal effect of the compounds in three Water Treatment Plants was calculated. The compounds studied were generally removed during conventional water treatment, especially during the active carbon filtration.

Fragrance Analysis Using GC-MS and Electronic Nose in Phalaenopsis (GC-MS와 전자코를 이용한 팔레놉시스 향기 분석)

  • Park, PueHee;Yae, ByeongWoo;Kim, MiSeon;Lee, YoungRan;Park, PilMan;Lee, DongSoo
    • FLOWER RESEARCH JOURNAL
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    • v.19 no.4
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    • pp.219-224
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    • 2011
  • Phalaenopsis (P.) has various species, and some of them have strong fragrance. There are fragrant species such as P. bellina, P. violacea, P. schilleriana and used in breeding program for fragrant Phalaenopsis. This study was performed for establishment of fragrance analysis system using GC-MS and electronic nose in eight P. resources. We analyzed fragrant compound using the tissue of sepal, petal, column, and lip of P. '3010'. The percentage of the major compound was high in the petal and lip tissues. The main compound emitted from P. bellina was linalool (21.21%). It was possible that fragrance pattern could be analyzed among the resources using the electronic nose. Discriminant function analysis (DFA) was more useful than the principal component analysis (PCA) in statistics program. We utilized GC-MS method for the major compounds of flower from our breeding materials. This study would be useful to the fragrant analysis system for the fragrant orchid breeding in the future.

Analysis of Binding Media in Dancheong Sample from Unhangak Hall of Hwaryeongjeon Shrine, Suwon (수원 화령전 운한각 단청시편의 교착제 분석)

  • Park, Jongseo;Lee, Sun Myung;Mun, Seong Woo;Kang, Yeong Seok
    • Journal of Conservation Science
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    • v.37 no.3
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    • pp.245-254
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    • 2021
  • In this study, organic materials in Dancheong specimens were analyzed to establish a Dancheong preparation method in Unhangak Hall of Hwaryeongjeon Shrine, Suwon. IR and pyrolysis/GC/MS were applied to a Zuhong specimen and a gilded one. The IR spectra showed absorption peaks corresponding to C-O, C=O, OH, although they were different from those of animal glue, Asian lacquer, and drying oil. The Pyrolysis/GC/MS after the on-line methylation revealed Asian lacquer-derived components, such as methyl 7-(2,3-dimethoxyphenyl)heptanoate, and drying oil-derived components, such as nonanedioic acid, dimethyl ester. Based on these results, we estimated that Asian lacquer and drying oil were used in the Dancheong preparation. Small amounts of 3-methyl-1H-pyrrole were also detected, which could possibly originate from animal glue. The radiocarbon age of the specimens appeared to be between the late 17th to the early 20th century. This study potentially reports the first case of Asian lacquer detection in a Dancheong specimen in Korea.

Comparative Study of Extracting Fragrance Allergens by GC-MS/MS

  • Lee, In Ja;Ahn, Jae-Chan;Kim, Bogsoon;Chung, Deukmo
    • Mass Spectrometry Letters
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    • v.8 no.1
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    • pp.18-22
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    • 2017
  • Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

Extractive Compounds of Ramaria formosa(Fr.) Quel (붉은싸리버섯의 추출성분)

  • 황병호;이태성
    • Journal of Korea Foresty Energy
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    • v.22 no.3
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    • pp.37-42
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    • 2003
  • To elucidate chemical strvacture of Ramaria formosa(Fr.) Quel was extracted with methanol for 72 hours, and then filtered twice. The extractive compounds were analyzed by the Libaries Search method, using GC and GC-MS Spectrometry. As a result, the five different compounds were analyzed, such as (1) methyl-hexadecanoate, (2) methyl-9,12- octadecadienoate, (3) methyl-cis-9-octadecenoate, (4) methyl-octadecanoate, and (5) 4-hexyl-2,5-dihydro-2,5-dioxo-3-furanacetic acid. The large quantity of compound, 4-hexyl-2,5-dihydro-2,5-dioxo-3-furanacetic acid, is expected that through experiments on animals the compound will be a potential agent which can be developed as a health food to relieve constipation or a laxative medicine.

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