• Title/Summary/Keyword: GC-MS analysis

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Multivariate Analysis and Gas Chromatographic Determination of the Smelly Nitro Compounds in Dried-Fishes (GC에 의한 건어물 냄새성분중 질소화합물 분석과 다변량해석)

  • Bae, Sun Young;Lee, Dong Sun
    • Journal of the Korean Chemical Society
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    • v.41 no.2
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    • pp.105-112
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    • 1997
  • The smelly nitro compounds were extracted from dried fishes by simultanous distillation and extraction, then were analyzed by GC-MS. Carbon number and order of an amine could be predicted by using retention time and equivalent chain length. Anchovy, codfish, imitation crab meat, cuttle fish, file fish, pollack, shrimp, octopus, harvest fish, and hard-shelled mussel were used for this investigation. Various smelly nitro compounds such as methylamine, acetamide, thiazole, 2-hydroxy isopropylamine, N-methyl pyrroline, piperidine, cyclohexylamine were identified, however, dimethylamine, trimethylamine, diethylamine were not detected. Principal components analysis was applied to GC-MS profiles for pattern recognition of smelly nitro compounds in dried fishes. Multivariate aspects using principal components analysis were very useful for pattern recognition of smelly components, category similarity.

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Multi-residue Analysis of Pesticides using GC-TOF/MS, ECD, NPD with QuEChERS Sample Preparation (QuEChERS 전처리법과 GC-TOF/MS, ECD, NPD를 이용한 잔류농약 다성분분석)

  • Park, Jungwook;Kim, Aekyung;Kim, Jongpil;Lee, Hyanghee;Park, Duckwoong;Moon, Sujin;Ha, Dongryong;Kim, Eunsun;Seo, Kyewon
    • The Korean Journal of Pesticide Science
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    • v.18 no.4
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    • pp.278-295
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    • 2014
  • Fast and accurate multi-residue pesticides inspecting method needs in Agro-Fishery Products Inspection Center. So, We tried to seek the optimum method using GC-TOF/MS, GC-ECD, GC-NPD after QuEChERS sample preparation. In GC-TOF/MS, 138 kinds of pesticide were spiked at 0.3 and $0.5{\mu}g/g$for the identification and quantification in lettuce sample. Recoveries of 77 pesticides were between 70 and 130% with RSD (relative standard deviation lower than 20% at $0.3{\mu}g/g$. In GC-ECD, NPD, 146 kinds of pesticide were spiked for the identification and quantification in lettuce. Recoveries of 61 species were between 70 and 130% with lower than 20%. These results indicated that GC-TOF/MS, GC-ECD, NPD analysis with the QuEChERS sample preparation can be partly applied to multi-residue pesticides in vegetables.

Analysis of ambers with different origin by IR and py/GC/MS (산지별 호박(amber)의 IR 및 py/GC/MS 특성 분석)

  • Park, Jong-Seo;Lim, Yu-Jin
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.256-265
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    • 2011
  • Ambers have been used as a gemstone and a religious object since the ancient times and found in several archaeological sites in Korea. To prepare an enhanced conservation measures, we surveyed the chemical and spectroscopic properties of the ambers according to the provenance. Total 14 amber samples were collected from 6 different provenances including Baltic, Chiapas, Colombian, Dominican, Fushun and Madagascar amber. Infrared (IR) spectroscopic analysis was conducted for the non-destructive examination of the amber samples. They were also analyzed with pyrolysis/GC/MS (py/GC/MS) at the pyrolysis temperature of $300^{\circ}C$ with the on-line derivatization to trimethylsilyl ester. Baltic shoulder corresponding to the absorption at $1250cm^{-1}{\sim}1150cm^{-1}$ appeared in the IR spectrum of Baltic amber. IR spectra of the other ambers also showed somewhat distinctive characteristic peaks. In py/GC/MS analysis peaks assignable to succinic acid, dehydroabietic acid and pimaric acid were detected, which are known to be the components of the amber. In the meanwhile, the presence of compounds appearing in certain amber will be applied to differentiate the provenances of amber relics if their fragments are available for the analysis. These results are expected to help the confirmation of archaeological amber relics and archaeometric interpretation of provenances and manufacturing techniques.

Geographical origin discrimination of Korean variety, Angelica gigas Nakai by using TDU (Thermal Desorption Unit)-GC/MS (TDU-GC/MS를 이용한 한국품종 참당귀 국산 판별 기법)

  • Lee, Mi-Na;Kim, Yoon-Suk;Kim, Won-Il;Kim, Jeong-Gyu;Kwon, Oh-Kyung
    • Journal of Applied Biological Chemistry
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    • v.63 no.1
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    • pp.29-33
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    • 2020
  • The objective of this study was to develop a fast and accurate method of variety discrimination and geographical discrimination origin of Korean angelica (Korean variety, Angelica gigas Nakai) by using TDU-GC/MS. Two peaks of decursin and decursinol, which are coumarin derivatives were identified in the range of Total Ion Chromatogram (TIC) RT 26.9-27.2 of the Korean angelica by GC/MS analysis at the time of condensation in a refrigerated condensation system after thermal desorption of sample extracts. In case of Chinese angelica (Chinese variety), ligustilide peak was detected at the RT 17.2. In order to investigate the difference of volatile components according to the geographical origin of Korean variety, the mass spectra were measured by TDU-GC/MS at the range of m/z 40-400 amu. The TIC of domestic cultivation and Chinese cultivation of the Korean variety, Angelica gigas Nakai showed the same tendency as a whole. However, in partial scans of TIC, two peaks detected at 15.54 and 16.05 of RT showed different peak patterns between Korean angelica (Korean variety) cultivated in Korea and in China. The ratio of Peak A (RT 15.54) and B (RT 16.05) was 0.0-0.2 for domestic cultivation and 0.5-2.8 for Chinese cultivation, confirming the possibility of discriminating origin by comparing the TIC peak pattern of TDU-GC/MS.

Organic Material Analysis of a Lacquered Wooden Sheath of Long Sword with Ring Pommel Excavated in Imdang Ancient Tomb (경산 임당고분 출토 철제 고리자루칼 칠의 유기물 분석)

  • Park, Jongseo;Cho, Ha-nui;Lee, Jae-sung
    • Journal of Conservation Science
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    • v.34 no.5
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    • pp.369-377
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    • 2018
  • In order to examine the constituents and weathered state of a lacquer specimen, analysis of the organic materials was conducted using py/GC/MS(pyrolysis-gas chromatography-mass spectrometry). The samples were obtained from the lacquered wooden sheath of a long ring-pommel sword excavated in the Imdang No.1 ancient tomb constructed around the Proto-Three Kingdoms period. In direct py/GC/MS, the sample and the dried Asian lacquer showed similar chromatograms, while the characteristic compounds of Asian lacquer such as 1,2-dimethoxy-3-pentadecylbenzene were observed in THM(thermally assisted hydrolysis and methylation)-py/GC/MS. In addition, compounds like dimethyl nonanedioate, which presumably originated from drying oil, were also detected. Furthermore, the detection of oxidized catechols in considerable amount indicated that the degradation of lacquer is estimated to result from the oxidation of urushiol. Therefore, it is suggested that the lacquered wooden sheath was prepared using Asian lacquer and drying oil, and that the lacquer layer was considerably oxidized over the long burial time.

Analysis of Cyclofenil and its Metabolites in Human Urine using GC/MS (GC/MS를 이용한 소변중의 Cyclofenil 및 그 대사체의 분석)

  • Myung, Seung-Woon;Min, Hye-Ki;Cho, Hyun-Woo;Kim, Dong-Hyun;Kim, Myungsoo
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.185-189
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    • 2002
  • International Olympic Committee (IOC) prohibits the use of cyclofenil for male. To prove whether cyclofenil product was taken or not, the analytical method in urine using GC/MS was established. The extraction recoveries of cyclofenil and its metabolites were higher in the range of pH 5-9. Because the parent drug (cyclofenil) was not excreted in urine, metabolites were detected and theses were used as a criteria of cyclofenil dose. Therefore the metabolites were hydrolyzed, extracted at pH 9.6, derivatized with MSTFA and analyzed by GC/MS.

Flavor Components of Poncirus trifoliata (탱자(Poncirus trifoliata)의 향기성분 분석에 관한 연구)

  • Oh, Chang-Hwan;Kim, Jung-Han;Kim, Kyoung-Rae;Ahn, Hey-Joon
    • Korean Journal of Food Science and Technology
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    • v.21 no.6
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    • pp.749-754
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    • 1989
  • The essential oil was prepared by a gas co-distillation method from flavedo of Poncirus trifoliata and was analyzed by GC/ retention index (RI) and GC/MS. The essential oil prepared by a gas co-distillation gave a whole fragrance of Poncirus trifoliata. The identification of the flavor components was performed by multi-dimensional analysis using GC/RI and GC/MS. GC/RI and GC/MS were complementary to each other. In applying GC/RI for identification, it was more effective when two columns of different polarities were used. Thirty volatile flavor constituents were identified in Poncirus trifoliata. Limonene, myrcene, ${\beta}-caryophyllene,\;trans-{\beta}-ocimene$, ${\beta}-pinene$, 3-thujene and 7-geranyloxycoumarin were the major constituents and cis-3-hexenyl acetate, n-hexyl acetate, 2-methyl acetophenone, elixene and elemicine had not been reported earlier as citrus components.

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Study on the analytical method using GC-MS for the accident preparedness substances (실험실 GC-MS를 이용한 사고대비물질 분석방법 연구)

  • Kim, Kijoon;Lee, Jinseon;Lee, Suyeong;Hwang, Seungryul;Kim, Younghee;Seok, Gwangseol
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.80-85
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    • 2013
  • The sixty nine accident preparedness substances (APS) having high probability of chemical accident are controlled under the Toxic Chemicals Control Act (TCCA). Around the world, there has been a growing interest in the analysis of chemical warfare agent (CWAs). When a chemical accident occurs, it is generally required to detect and identify APS. However, the quantitative analytical data remain limited in Korea. In this study, an analytical method using GC/MS for volatile organic chemicals was established and a quantitative analysis method was studied. The calibration curve for 25 chemicals were obtained and 21 chemicals showed higher coefficient of determination ($r^2$ >0.998).

Analysis of Lacquer and CNSL Using Infrared Spectrometer and Pyrolysis-GC/MS (적외선분광분석과 Py-GC/MS를 이용한 옻칠 및 캐슈칠도막 분석)

  • Choi, Jaewan;Kim, Soo-Chul
    • Journal of the Korean Wood Science and Technology
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    • v.46 no.1
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    • pp.1-9
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    • 2018
  • Nowadays, synthetic resin varnish such as cashew nut shell liquid (CNSL) is being used as well as traditional lacquer. The code of ethics states that material must be identical to the original when preserving cultural heritage. Therefore, lacquer should be used. However, problem is that even experts have difficulties differentiating lacquer and CNSL as they have similar components. Therefore, this study was carried out to identify the difference between lacquer and CNSL using IR and Py-GC/MS. As a result of IR, in lacquer, $720cm^{-1}$ peak was detected and in CNSL, $750cm^{-1}$, $720cm^{-1}$ and $700cm^{-1}$ peaks were detected. The results of Py-GC/MS detect benzene compounds and alkyl chains for both varnishes. However, hexanoic acid was detected from CNSL but not lacquer. Using these analytical methods, the differences between lacquer and CNSL can be identified on the scene. This is expected to be applied to the authentic conservation and restoration of lacquerware.

Determination of Methylmercury in Biological Samples Using Dithizone Extraction Method Followed by Purge & Trap GC-MS

  • Lee, Jung-Sub;Ryu, Yoon-Jung;Park, Jae-Sung;Jeon, Sung-Hwan;Kim, Sam-Cwan;Kim, Young-Hee
    • Bulletin of the Korean Chemical Society
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    • v.28 no.12
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    • pp.2293-2298
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    • 2007
  • In this study, a dithizone extraction technique involving purge & trap GC-MS was developed for the determination of methylmercury in biological samples, especially blood and fish. After alkaline digestion, methylmercury in biological samples was extracted into dithizone and back-extracted into aqueous sulfide solution. The extracted methylmercury was converted to the volatile ethyl derivative, purged and trapped onto a solid-phase collection medium, and then introduced into the GC-MS system. The determined MDLs of the established method were 0.9 ng·g?1 for biological samples and its accuracy and precision were found to be 93% and 3.8%, respectively. The method was validated by analysis of CRMs such as SRM 966, BCR 463 and IAEA 407 and all analytical results were within certified ranges with average RSDs of less than 6%. The analytical results of field-sampled fish also showed that the method can be successfully used as an alternative for commonly used distillation method followed by GC-CVAFS detection.