• 제목/요약/키워드: Gas chromatography-mass spectrometry (GC/MS)

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Formation of Pyro-products by the Pyrolysis of Monobromophenols

  • Na, Yun-Cheol;Seo, Jung-Ju;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제24권9호
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    • pp.1276-1280
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    • 2003
  • Thermal behavior of bromphenols was investigated by direct pyrolysis at high temperature. The thermal degradation products formed by the pyrolysis of mono-bromophenols (o-, m-, and p-) were identified by gas chromatography-mass spectrometry. During the pyrolysis reactions, several kinds of dioxins and furans were produced, and the relative ratio of pyro-products was dependent on the substituted position of bromine in phenolic structure due to the effect of symmetry and steric hindrance. The formation of dioxins can be explained by the phenoxy radical addition and Br atom elimination at an ortho-carbon site on phenolic structure. On the other hand, the formation of furans can be explained by the ortho-ortho carbon coupling of phenoxy radicals at unsubstituted sites to form o, o'-dihydroxydiphenyl intermediate via its keto-tautomer, followed by $H_2O$ elimination. The pyrolysis temperature has also a substantial effect on the dimerized products quantities but little effect on the type of pyro-products. Moreover, the formation mechanism of pyro-products was suggested on the basis of products identified.

Sensitive Determination of Natural and Synthetic Steroidal Hormones of a Free and Conjugated Form in Surface Water by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Oh, Jin-Aa;Shin, Sun-Kyoung
    • Bulletin of the Korean Chemical Society
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    • 제32권3호
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    • pp.809-814
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    • 2011
  • A method based on the TMS derivatives and acidic hydrolysis was developed for the simultaneous determination of free and conjugated steroidal hormones in surface water. A silylation of five natural and two synthetic steroidal hormones was achieved with N-methyl-N-(trimethylsilyl) trifluoroacetamide/$NH_4I$ (1000:3) under catalysis of dithioerythritol for 60 min at $80^{\circ}C$. TMS derivatives of the steroid hormones containing multifunctional groups offer a single derivative product under this condition. The accuracy of the analytes was in the range of 87 to 110% at a concentration of 20 and 50 ng/L with relative standard deviations of less than 10%. The method detection limit was in the range of 0.01 to 0.02 ng/L for surface water. Natural steroidal hormones were detected in a concentration range of 0 to 1.03 ng/L in free form and 0 to 14.6 ng/L in conjugated form, respectively. We found that most of the natural hormonal steroids exist in conjugate forms (43 to 100%) in river water.

AEDA법에 의한 한국산 젓갈류의 Aroma-Active 성분의 구명 1. 시판 멸치젓의 Aroma-Active 성분 (Identification of Aroma-Active Compounds in Korean Salt-Fermentaed Fishes by Aroma Extract Dilution Analysis 1. Aroma-Active Components in Salt-Fermented Anchovy on the Market)

  • 차용준;김훈;장성민;박지영
    • 한국식품영양과학회지
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    • 제28권2호
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    • pp.312-318
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    • 1999
  • Volatile compounds in salt fermented anchovy on the market were analyzed by vacuum simulta neous distillation solvent extraction/gas chromatography/mass spectrometry/olfactometry(V SDE/ GC/MS/O) and aroma extract dilution anlaysis(AEDA). Predominant odorants(Log3FD$\geq$8) in sample were ethyl methylbutanoate(candy like/sweet) and 2 ethyl 3,5 dimethylpyrazine(nutty/baked potato like). Besides these compounds, 6 odorants such as ethyl 3 methylbutanoate(sweet/floral/ candy like), 3 methylbutanal(dark chocolate like), (Z) 4 heptenal(rancid/fish like), (methylthio) propanal(soy sauce /baked potato like), (E,Z) 2,6 nonadienal(melon /cucumber like) and (E,E) 2,4 decadienal(fatty/cooked soybean like) were potent in odor value of salt fermented anchovy. Seven amino acids having high taste value in sample were glutamic acid, aspartic acid(sour and umami taste), lysine, alanine(sweet), histidine, valine, and methionine(bitter).

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Essential Oil Constituents of Swertia chirata Buch.-Ham.

  • Gyawali, Rajendra;Ryu, Keun-Young;Shim, Sung-Lye;Kim, Jun-Hyoung;Seo, Hye-Young;Han, Kyu-Jae;Kim, Kyong-Su
    • Preventive Nutrition and Food Science
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    • 제11권3호
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    • pp.232-236
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    • 2006
  • The essential oil of Swertia chirata Buch.-Ham. was extracted by solvent extraction (n-pentane:diethylether, 1:1) method using simultaneous distillation-extraction (SDE) apparatus and analyzed by gas chromatography-mass spectrometry (GC/MS). The yield of essential oil obtained from S. chirata was 236.47 mg/kg. Seventy seven compounds of the essential oil belonging to chemical classes of acid (4), alcohol (21), aldehyde (15), ester (3), furan (3), hydrocarbon (7), ketone (17) and miscellaneous (7) were tentatively identified. The major volatile compounds ranged in content order were as follows: undecanoic acid (28.63%), 2-buten-2-one (20.42%), camphor (18.40%), 2-heptadecanone (14.72%), and cedrol (13.07%).

Rapid Determination of Volatile Organic Compounds in Human Whole Blood Using Static Headspace Sampling with Gas Chromatography and Mass Spectrometry

  • Lee, Ji-Young;Kim, Seungki;Lee, Jong-Tae;Choi, Jong-Ho;Lee, Jeongae;Pyo, Heesoo
    • Bulletin of the Korean Chemical Society
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    • 제33권12호
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    • pp.3963-3970
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    • 2012
  • Headspace (HS) and headspace solid-phase microextraction (HS-SPME) were studied for extracting volatile organic compounds (VOCs) from whole blood, with chemical and instrumental variables being optimized for maximum sensitivity: incubation at $60^{\circ}C$, equilibration for 30 min, pH 11, and 2 mL injection volume. Both techniques provided accurate analyses, with detection limits of 0.05-0.1 ng $mL^{-1}$ and 0.05-0.5 ng $mL^{-1}$. HS showed better sensitivity, reproducibility, and analysis times than HS-SPME. Overall levels of chloroform in whole blood were found to be 0.05-5.84 ng $mL^{-1}$; detected levels of benzene were 0.05-2.20 ng $mL^{-1}$.

Synthesis and Application of Metal Doped Silica Particles for Adsorptive Desulphurization of Fuels

  • Jabeen, Bushra;Rafique, Uzaira
    • Environmental Engineering Research
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    • 제19권3호
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    • pp.205-214
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    • 2014
  • Petroleum a vital commodity affecting every aspect of 21st century. Toxicity and adverse effects of sulphur as catalyst in petroleum products is of great concern required development of techniques for desulphurization in compliance with the International standards. Installation of desulphurizing units costs over $200 million per unit placing economic burden on developing countries like Pakistan. Present study analysis of commercial fuels (station petrol and jet fuel JP8) on gas chromatography-mass spectrometry (GC-MS) identified sulphur concentration of 19.94 mg/L and 21.75 mg/L, respectively. This scenario urged the researcher to attempt synthesis of material that is likely to offer good adsorption capacity for sulphur. Following protocol of sol-gel method, transition metals (Ni, Cu, Zn) solution is gelated with tetraethoxysilane (TEOS; silica precursor) using glycerol. Fourier transform infrared spectroscopy (FTIR) spectra revealed bonding of Zn-O, Cu-O, and Ni-O by stretching vibrations at $468cm^{-1}$, $617cm^{-1}$, and $468cm^{-1}$, respectively. Thiophene and Benzothiophene mixed in n-heptane and benzene (4:1) for preparation of Model Fuels I and II, respectively. Each of silica based metal was applied as adsorbent in batch mode to assess the removal efficiency. Results demonstrated optimal desulphurization of more than 90% following efficacy order as Si-Ni > Si-Zn > Si-Cu based adsorbents. Proposed multilayered (Freundlich) adsorption mechanism follows ${\pi}$-complexation with pseudo secnd order kinetics.

Chemical Constituents of Essential Oils Possessing Anti-Influenza A/WS/33 Virus Activity

  • Choi, Hwa-Jung
    • Osong Public Health and Research Perspectives
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    • 제9권6호
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    • pp.348-353
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    • 2018
  • Objectives: This study was conducted to determine whether essential oils had anti-influenza A/WS/33 virus activity and whether there were specific compounds associated with this activity. Methods: There were 63 essential oils evaluated for anti-influenza (A/WS/33 virus) activity using a cytopathic effect reduction method. The chemical composition of the anti-influenza essential oils was phytochemically analyzed by gas chromatography-mass spectrometry. Results: The antiviral assays demonstrated that 11 of the 62 essential oils ($100{\mu}g/mL$) possessed anti-influenza activity, reducing visible cytopathic effects of influenza A/WS/33 virus activity by > 30%. Furthermore, marjoram, clary sage and anise oils exhibited anti-influenza A/WS/33 virus activity of > 52.8%. However, oseltamivir (the anti-influenza A and B drug), showed cytotoxicity at the same concentration ($100{\mu}g/mL$) as the essential oils. The chemical composition detected by GC-MS analysis, differed amongst the 3 most potent anti-viral essential oils (marjoram, clary sage and anise oils) except for linalool, which was detected in all 3 essential oils. Conclusion: This study demonstrated anti-influenza activity in 11 essential oils tested, with marjoram, clary sage and anise essential oils being the most effective at reducing visible cytopathic effects of the A/WS/33 virus. All 3 oils contained linalool, suggesting that this may have anti-influenza activity. Further investigation is needed to characterize the antiviral activity of linalool against influenza A/WS/33 virus.

Pyrolysis Properties of Lignins Extracted from Different Biorefinery Processes

  • Lee, Hyung Won;Jeong, Hanseob;Ju, Young-Min;Youe, Won-Jae;Lee, Jaejung;Lee, Soo Min
    • Journal of the Korean Wood Science and Technology
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    • 제47권4호
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    • pp.486-497
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    • 2019
  • The non-isothermal and isothermal pyrolysis properties of H lignin and P lignin extracted from different biorefinery processes (such as supercritical water hydrolysis and fast pyrolysis) were studied using thermogravimetry analysis (TGA) and pyrolyzer-gas chromatography/mass spectrometry (Py-GC/MS). The lignins were characterized by ultimate/proximate analysis, FT-IR and GPC. Based on the thermogravimetry (TG) and derivative thermogravimetry (DTG) curves, the thermal decomposition stages were obtained and the pyrolysis products were analyzed at each thermal decomposition stage of non-isothermal pyrolysis. The isothermal pyrolysis of lignins was also carried out at 400, 500, and $600^{\circ}C$ to investigate the pyrolysis product distribution at each temperature. In non-isothermal pyrolysis, P lignin recovered from a fast pyrolysis process started to decompose and produced pyrolysis products at a lower temperature than H lignin recovered from a supercritical water hydrolysis process. In isothermal pyrolysis, guaiacyl and syringyl type were the major pyrolysis products at every temperature, while the amounts of p-hydroxyphenyl type and aromatic hydrocarbons increased with the pyrolysis temperature.

케로신 연료의 침탄 특성에 대한 온도의 영향 (Effects of Temperature on the Coking Characteristics of Kerosene)

  • 김민철;김영진;김정수
    • 한국추진공학회지
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    • 제23권2호
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    • pp.46-52
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    • 2019
  • 케로신 연료의 침탄 특성에 대한 온도의 영향을 분석한 실험이 수행되었다. 케로신을 각각 600 K, 700 K, 800 K으로 가열한 후, 냉각시킨 시료를 채취하였다. 사용된 구리관은 온도조건에 따라 새로이 교체했다. 기체 크로마토그래피-질량분석과 에너지분산형 X선 분광기가 장착된 주사전자현미경을 통해 액체 시료와 구리 시편의 침탄 특성을 각각 분석하였다. 그 결과, 비교적 고온(800 K)으로 가열된 구리 시편의 내부표면에서 연료의 침탄으로 인해 침전물이 발생한 것을 확인하였다.

Hydrophilic Extracts of the Bark from Six Pinus Species

  • Masendra, Masendra;Ashitani, Tatsuya;Takahashi, Koetsu;Susanto, Mudji;Lukmandaru, Ganis
    • Journal of the Korean Wood Science and Technology
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    • 제47권1호
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    • pp.80-89
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    • 2019
  • Pine barks are important biomass resources because they are utilised in the production of pine wood and rosins. However, no chemical study has been conducted on the hydrophilic status of pine barks in Indonesia. This aim of this study is to explore the hydrophilic extracts of the barks from six Pinus species (P. elliotii, P. caribeae, P. oocarpa, P. merkusii P. montezumae, and P. insularis). The hydrophilics of pine barks were analysed using gas chromatography-mass spectrometry. The presence of polyphenol contents in the ethanol extracts obtained from the barks of six Pinus species was determined using the tannin-formaldehyde method, Folin-Cioucalteu assay, and vanillin-HCl assay. The ethanol and hot water soluble extractives derived from inner barks were higher in quantity when compared to those derived from the outer bark samples. The polyphenol measurement showed that the highest value of total phenol content was derived from the outer bark of P. montezumae whereas those of the total phenol and tannin- formaldehyde contents were derived from the inner and outer barks of P. oocarpa. GC-MS analysis revealed that nitrogenous compounds are dominant constituents in the inner and outer barks of the six species, followed by sugars and monophenolics, respectively.