• Title/Summary/Keyword: headspace GC-MS

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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.

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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    • v.33 no.12
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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 $mL^{-1}$.

Examination about evaluation method of odor active compounds in evaporator by using condensed water (응축수를 이용한 냉각기의 냄새원인물질 평가방법 검토)

  • Kim, Sun-Hwa;Kim, Kyung-Hwan;Jung, Young-Rim;Kim, Man-Goo;Kim, Jae-Ho;Park, Ha-Young;Ji, Yong-Jun
    • Analytical Science and Technology
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    • v.20 no.5
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    • pp.361-369
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    • 2007
  • Uncomfortable odor emitted from air conditioning system is the main cause of indoor air quality deterioration. To solve evaporator odor problems, odor active compounds, have to be identified then the quality of the product can be improved its quality. Because evaporator odor in exhaust gas has low odor intensity and discontinuity, it is very difficult to collect and analyze sample. In this study through the identification of odor compounds in condensed water, the evaluation of the eraporator was tested. Odor compounds were extracted from water by headspace-solid-phase microextraction (HS-SPME) method. The single odor was separated by GC/FID/Olfactometry (GC/FID/O) and odor active compounds were identified by GC/AED and GC/MS. Compared to air sample, result of sensory evaluation and the single odor compound appeared similarly. It was identified that odor active compounds have functional group containing oxygen such as alcohols and acids. Evaluation method of odor active compounds using condensed water in evaporator appeared effective on the side of simplicity of collection, low expanse and rapid analysis.

Composition and Cytotoxicity of Essential Oil from Korean rhododendron (Rhododendon mucronulatum Turcz. var. ciliatum Nakai) (털진달래(Rhododendon mucronulatum Turcz. var. ciliatum Nakai) 정유의 성분분석과 독성평가)

  • Park, Yu-Hwa;Kim, Song-Mun
    • Applied Biological Chemistry
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    • v.51 no.3
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    • pp.233-237
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    • 2008
  • The essential oil was obtained from the aerial part of Rhododendon mucronulatum Turcz. var. ciliatum Nakai by steam distillation, samples were collected by headspace (HS) and solid-phase microextraction (SPME) methods, and the compositions of the oil were analyzed by gas chromatography-mass spectrometry (GC-MS). Nineteen constituents were identified from the essential oil: 15 carbohydrates, 3 alcohols, and 1 acetates. Major constituents were 2-${\beta}$-pinene (16.1%), camphene (11.9%), ${\delta}$-3-carene (11.4%), d,l-limonene (9.5%), and ${\gamma}$-terpinene (9.5%). By SPME extraction, seventeen constituents were identified: 13 hydrocarbons, 1 alcohol, 1 nitrogen-containing compound, 1 acetate, and 1 amine. Major constituents of the SPME-extracted sample were cam phene (19.6%), 2-${\beta}$-pinene (18.0%), ${\delta}$-3-carene (17.4%), trimethyl hydrazine (9.7%), ${\gamma}$-terpinene (8.5%), and d,l-limonene (5.5%). By HS extraction, thirteen constituents were identified: 11 hydrocarbons, 1 alcohol, and 1 nitrogen-containing compound. Major constituents of the HS-extracted sample were camphene (25.8%), ${\delta}$-3-carene (24.8%), 2-${\beta}$-pinene (20.2%), d,l-limonene (5.4%), tricyclene (5.1%) and trimethyl hydrazine (4.6%). The fragrance of the essential oil was coniferous, balsamic, and woody, and the $IC_{50}$ value of the essential oil was 0.030 ${\mu}g/mg$ in MTT assay using UaCaT keratinocyte cell line.

Simultaneous determination of 37 volatile organic compounds at ng/L concentration level in surface water by HS-SPME-GC/MS (HS-SPME-GC/MS에 의한 지표수에서 ng/L 농도 수준의 37개 휘발성유기화합물의 동시 분석)

  • Kim, Tae-Seung;Hong, Suk-Young;Kim, Jong-Eun;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.39-49
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    • 2012
  • A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

Analysis of Volatile Flavor Components of Pleurospermum kamtschaticum (누룩치의 휘발성 향미성분 분석)

  • 정미숙;이미순
    • Korean journal of food and cookery science
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    • v.14 no.5
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    • pp.541-546
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    • 1998
  • Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.

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Identification of Flavor Components in Tomato Fruit (토마토 향기성분의 동정)

  • Sohn, Tae-Hwa;Cheon, Sung-Ho;Choi, Sang-Won;Moon, Kwang-Deok
    • Applied Biological Chemistry
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    • v.31 no.3
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    • pp.292-297
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    • 1988
  • The volatiles of whole and homogenated tomato fruits collected by the headspace trapping method using Tenax GC and the simultaneous steam distillation method were identified by GC and GC-MS. Among over 100 GC peaks, 10 alcohols, 6 aldehydes, 4 ketones, 3 esters, 1 phenol and 1 acid were identified from whole tomato fruits, whereas 12 alcohols, 6 aldehydes, 5 ketones, 5 esters, 2 phenols, 1 hydrocarbon and 1 acid were identified from homogenated tomato fruits. By simultaneous steam distillation-extraction, 19 alcohols, 13 hydrocarbons, 9 esters, 9 ketones, 8 aldehydes, 2 phenols, 2 lactones,2 furans, 1 acids and 2 others were identified among over 300 peaks.

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Effects of fermentation by the commercial starter ABT-5 on the flavor and antioxidant activities of dark chocolate (복합 유산균 스타터 ABT-5를 이용한 발효 다크 초콜릿의 항산화 활성 및 향기 성분)

  • Koh, So Yae;Ryu, Ji-Yeon;Kim, Hyeon A;Kim Cho, Somi
    • Korean Journal of Food Science and Technology
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    • v.49 no.6
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    • pp.617-624
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    • 2017
  • Chocolate, one of the most popular confectioneries in the world, is known for its aromatic flavor and high antioxidant activities. In this study, we investigated the effects of fermentation with commercially available lactic acid bacteria, ABT-5, on the flavor and antioxidant activities of dark chocolate. During 24 h fermentation, pH decreased from 5.52 to 3.97 and total acidity increased from 0.51 to 1.85%, whereas total polyphenol and flavonoid contents as well as DPPH and ABTS radical scavenging activities remained unchanged. Furthermore, compared with control HepG2 cells treated with unfermented dark chocolate, those treated with the fermented dark chocolate showed significantly lower levels of reactive oxygen species and higher viability under $H_2O_2-induced$ oxidative stress. Finally, GC-MS and headspace GC-MS analysis detected 4-hydroxy-2,5-dimethyl-3(2H)-furanone and 2-furanmethanol, known to enhance flavor, in the fermented dark chocolate. Collectively, these results suggest that ABT-5-fermented dark chocolate could be utilized for developing value-added dark chocolate products.

Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Analysis of Flavor Composition of Coriander Seeds by Headspace Mulberry Paper Bag Micro-Solid Phase Extraction

  • Cha, Eun-Ju;Won, Mi-Mi;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2675-2679
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    • 2009
  • This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.