• Title/Summary/Keyword: GC/MS spectrometry

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Analysis of volatile compounds and metals in essential oil and solvent extracts of Amomi Fructus (사인으로부터 추출한 정유와 용매 추출물의 휘발성 물질 및 금속성분 분석)

  • Lee, Sam-Keun;Eum, Chul Hun;Son, Chang-Gue
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.436-445
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    • 2015
  • Amomi Fructus with anti-oxidative activity was chosen and essential oil was obtained by SDE (simultaneous distillation extraction), and 39 constituents were determined by GC-MS (gas chromatography-mass spectrometry). Major components were camphor, borneol acetate, borneol, D-limonene and camphene. Three solvent extracts such as hexanes, diethyl ether and methylene chloride from Amomi Fructus were obtained. These were analyzed by GC-MS and 4 more constituents were identified in addition to 39 components discovered in essential oil. Five major components such as camphor, borneol acetate, borneol, D-limonene and camphene were also detected, however the relative peak percents of those components were different from those of constituents in essential oil. To estimate the kind and the amount of materials evaporated at certain temperature and conditions from essential oil and solvent extracts, dynamic headspace apparatus was used and materials evaporated and trapped at certain conditions were analyzed by GC-MS. Recovery yield of SDE method from Amomi Fructus was measured by using camphor and standard calibration solution of camphor methanol solution and, the yield was 82.0%. Content of Hg was measured by mercury analyzer and contents of Cd, Pb, Cr, Mn, Co, Ni, Cu and Zn in Amomi Fructus, essential oils and solvent extracts were determined by ICP-MS (Inductively coupled plasma-mass spectrometer). Pb, Cd and Hg were measured in the concentration of 0.72 mg/kg, <0.10 mg/kg and 0.0023 mg/kg, respectively and these were below permission level of purity test. Contents of Mn, Cu and Zn in Amomi Fructus were 213 mg/kg, 8.29 mg/kg and 31.0 mg/kg, respectively and which were relatively higher than other metals such as Cr, Co and Ni. Metals such as Mn (0.65 ~ 9.08 mg/kg), Cu (1.16 ~ 4.40 mg/kg) and Zn (1.10 ~ 3.80 mg/kg) in essential oil and solvent extracts were detected. At this point it is not clear that the metals were cross-contaminated in the course of treating Amomi Fructus or metals were contained in Amomi Fructus. The influence evaluation toward biological model study of these metals in essential oil and solvent extracts will be needed.

Determination of the presence of benzene in vitamin drinks using headspace - solid phase microextraction and gas chromatography - mass spectrometry (Headspace Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry를 이용한 비타민드링크 제품 중 Benzene의 미량분석)

  • Kim, Jong-Hun;Lee, Kyung-Min
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.237-245
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    • 2007
  • The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

Comparative Sampling Procedures for the Volatile Flavor Components of Codonopsis lanceolata (전처리 방법에 따른 더덕(Codonopsis lanceolata)의 휘발성 향기성분 비교 분석)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Kim, Jae-Jung;Oh, Chang-Hwan
    • Korean Journal of Food Science and Technology
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    • v.24 no.2
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    • pp.171-176
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    • 1992
  • Volatile flavor components of Codonopsis lanceolata were extracted by gas co-distillation (GCD), solvent extraction/fractionation (SEF), and headspace sampling (HSS) methods. The extracts were analyzed by dual-capillary gas chromatography-retention index (GC-RI) and gas chromatography-mass spectrometry(GC-MS). The two extracts prepared by SEF and HSS gave more similar fragrance to the Codonopsis lanceolata than the GCD extract. The GC profiles of the SEF and HSS extracts were similar to each other except for differences in peak areas. The extract prepared by SEF gave a sweet note while the extract prepared by HSS gave a green note. The GCD extract began to give a burnt note of herb medicine with prolonged distillation. Rapid extraction of flavor components from Codonopsis lanceolata was possible in several short steps by SEF and HSS methods compared to GCD. GC-MS and GC-RI were used for peak identification. GC-RI was more effective for identification of isomers, and polar FFAP column was more suitable for identification of polar compounds. From Codonopsis lanceolata we identified 35 volatile flavor constituents, 24 of which have not been previously reported by simultaneous distillation extraction method $^{(5)}$. trans-2-Hexanal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, and hexanol were considered key components of the green note and 1-octen-3-ol, the component of the fresh note. Esters, including amyl propionate, seem to be responsible for the sweet note particular to Codonopsis lanceolata.

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Comparison of isoBOC derivatives, TBDMS derivatives, with US EPA Method in the sensitivity of Alkylphenols, Chlorophenols, and Bisphenol A potential field-screening applications of GC/MS-SIM

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.235.2-236
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    • 2002
  • The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring mode followed by three work-up methods for comparison: EPA method, isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in water samples were extracted with dichloromethane. (omitted)

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Studies on the Volatile Flavor Components of Fresh Ginseng (수삼중 휘발성 향기성분에 관한 연구)

  • 김만욱;박종대
    • Journal of Ginseng Research
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    • v.8 no.1
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    • pp.22-31
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    • 1984
  • Volatile flavor components of fresh ginseng (Panax ginseng C.A. Meyer.) were studied. Steam distillate of fresh ginseng was extracted with ethyl ether and the extract was separated into four fraction: neutral, phenolic, acidic and basis fractions. The ethyl ether concentrates and neutral fraction were analyzed by a combination of SE-54 fused silica capillary gas chromatography and mass spectrometry. Major flavor components of fresh ginseng were predominantly mono(n +2) and sesquiterpenes(n +3) in over two hundred constituents. Of these, 28 were newly identified in volatile flavor components of fresh ginseng by GC-MS.

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Formation of Polychlorinated Dibenzo-p-Dioxins and Their Thermal Decomposition Products from Pyrolysis Reactions of Chlorophenates

  • Hong, Jongki;Park, Jongsei;Kim, Kang-Jin
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.821-827
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    • 1995
  • Polychlorodibenzo-p-dioxins(PCDDs) have been prepared by microsacale pyrolysis of trichlorophenates. During the pyrolysis reaction, dechlorinated dibenzo-p-dioxins were also formed by the thermolysis of PCDDs. The dechlorination pathways of PCDDs were suggested in this reaction. The identification of these products was performed using capillary column gas chromatography-mass spectrometry.

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Volatile Flavor Components in Green Tea Blended with Parched Naked Barley (볶은 쌀보리를 혼합한 녹차의 휘발성 향기성분)

  • Choi, Sung-Hee
    • Journal of Life Science
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    • v.22 no.7
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    • pp.981-986
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    • 2012
  • To produce a new tea with a good flavor and functional properties using green tea of low quality, naked barley and barley were selected to blend with the green tea. The simultaneous distillation extraction method (SDE) using Likens and Nickerson's extraction apparatus was used to extract the volatile flavor compounds from the samples. The concentrated flavor extracts were analyzed and identified by GC and GC-MS. The GC patterns of the flavor components in two parched barleys were very different. The main volatile flavor components in two of the samples were alkyl pyrazines. Compounds including 3-methylbutanal, 2-methylbutanal, dihydro-2-methyl-3(2H)-furanone, 2,5-dimethyl pyrazine, and 3-ethyl-2.5-dimethyl pyrazine were isolated from the naked barley. Compounds including thiophenes, thiazoles, sulfides, and pyrroles with burnt odor were isolated from the barley. The parched naked barley was better than barley for adding to green tea. The main aroma components of the green tea blended with the naked barley were hexanol, hexanal, trans-2-hexenal, ${\beta}$-ionone, ${\alpha}$-ionone, alkyl pyrazines, 3-methylbutanal, 2-methylbutanal, and furfural.

Analysis of Volatile Components of a Chicken Model Food System in Retortable Pouches (레토르트 파우치 계육 모형식품의 휘발성분 분석)

  • Choi, Jun-Bong;Chung, Ha-Yull;Kong, Un-Young;Moon, Tae-Wha
    • Korean Journal of Food Science and Technology
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    • v.28 no.4
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    • pp.772-778
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    • 1996
  • In order to investigate changes of flavor during food sterilization in retortable pluches, a model food system consisting of 50% chicken breast meat, 1% salt and 49% chicken stock was analyzed before and after retorting using GC and GC-MS. In the analysis of the volatile components collected by the nitrogen purge and trap technique before and after retorting, a total of 53 peaks were observed on chromatograms and 42 peaks were identified. Among the 42 peaks identified were 17 caused by aldehydes, 9 by hydrocarbons, 8 by alcohols, 6 by ketones, 1 by furan and 1 by terpene. Analysis of the data obtained from our model food system strongly suggested that the compounds responsible for retort flavor are 2-heptanone, 2-pentyl furan and various ketones.

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Volatile flavor components of Korean ginger(Zingiber officinale Roscoe)extracted with liquid carbon dioxide (액체 이산화탄소 추출법에 의한 생강 (Zingiber officinale Roscoe)의 향기성분)

  • Kim, Myung-Kon;Na, Mun-Su;Hong, Jai-Sik;Jung, Soon-Taek
    • Applied Biological Chemistry
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    • v.35 no.1
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    • pp.55-63
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    • 1992
  • The essential oil of Korean ginger(Zingiber officinale Roscoe) was isolated by liquid carbon dioxide extraction method and fractionated into one hydrocarbon fraction and two oxygenated hydrocarbon fractions by using silica gel column chromatography. The compositions of the resulting oils were investigated by GC and GC-MS spectrometry. Out of 102 identified compounds, 44 were identified by comparing GC retention time and mass spectral data with authentic samples and 58 were tentatively identified according to mass spectral data only. The major compounds of hydrocarhon fraction were $zingiberene,\;{\beta}-sesquiphellandrene,\;{\gamma}-bisabolene,\;{\gamma}-cardinene,\;ar-curcumene$, and those of oxygenated hydrocarbon fractions wee geranal, sesquisabinene hydrate, borneol and zingiberenol. The major compounds of ginger oil were zingiberene, $citronellol+{\beta}-sesquiphellandrene,\;geranial,\;{\gamma}-bisabolene\;and\;ar-curcumene+geranyl\;acetate$, and ginger oil contained higher amounts of sesquiterpene hydrocarbons. The yield of extract was 6.96%.

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Determination of Residue Levels of Ethyl Carbamate in Alcoholic Beverages by Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS) (가스크로마토그래피/질량분석기(GC/MS/MS)를 이용한 주류 중 에틸카바메이트 잔류량 조사)

  • Kim, Dong-Ho;Jang, Han-Sub;Choi, Gu-Il;Kim, Hyun-Jung;Kim, Ho-Jin;Kim, Hyo-Lin;Kim, Keun-Sung
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.63-68
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    • 2013
  • Ethyl carbamate (EC) is a contaminant generated in the fermentation processes of various fermented foods. In this study, residue levels of EC in 95 alcoholic beverage samples were determined by using Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS). All the samples were purified by a liquid-liquid extraction (LLE) method using dichloromethane. The LLE method enables an improvement in time and cost to detection and specificity over the conventional extraction methods. The limits of detection and quantification (LOD and LOQ) to analyze EC were 1.3 and 4.0 ng/mL, respectively. The recovery rates of EC were ranged from 90.0 to 97.5% at the levels of 50, 100, and 500 ug/L. Among traditional grain-based alcoholic beverage samples (n = 34), the average residue levels of EC in takju, yakju, and cheongju were 0.63, 7.01, and 14.11 ug/L, respectively. Among fruit-based alcoholic beverage samples (n = 48), those of EC in japanese apricot spirits, bokbunjaju, grape wines, and other fruit wines were 79.18, 1.66, 2.64, and 2.39 ug/L, respectively. Among distilled or diluted alcoholic beverage samples (n = 13), those of EC in soju (distilled or diluted), general distillates, liquors, and brandies were 0, 3.30, 8.20, and 8.52 ug/L, respectively. Therefore, this study reports that the residue levels of EC in the alcoholic beverages, distributed in the current domestic markets, did not reach its maximum allowed levels of 30 and 400 ug/L established for grape and fruit wines in Canada, respectively.