• Title/Summary/Keyword: headspace-gas chromatography

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Headspace-Solid Phase Microextraction (HS-SPME) Analysis of Korean Fermented Soybean Pastes

  • Lee, Seung-Joo
    • Food Science and Biotechnology
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    • v.18 no.3
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    • pp.700-705
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    • 2009
  • In this study, the volatile compounds in 9 commercial fermented soybean pastes were extracted and analyzed by headspace-solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS), respectively. A total of 63 volatile components, including 21 esters, 7 alcohols, 7 acids, 8 pyrazines, 5 volatile phenols, 3 ketones, 6 aldehydes, and 6 miscellaneous compounds, were identified. Esters, acids, and pyrazines were the largest groups among the quantified volatiles. About 50% of the total quantified volatile material was contributed by 5 compounds in 9 soybean paste samples; ethyl hexadecanoate, acetic acid, butanoic acid, 2/3-methyl butanoic acid, and tetramethyl-pyrazine. Three samples (CJW, SIN, and HAE) made by Aspergillus oryzae inoculation showed similar volatile patterns as shown in principal component analyses to GC-MS data sets, which showed higher levels in ethyl esters and 2-methoxy-4-vinylphenol. Traditional fermented soybean pastes showed overall higher levels in pyrazines and acids contents.

Volatile Flavor Composition of White-flowered Lotus by Solid-phase Microextraction (Solid-Phase Microextraction에 의한 백련의 휘발성 향기 성분 분석)

  • Choi, Hyang-Sook
    • The Korean Journal of Food And Nutrition
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    • v.30 no.2
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    • pp.363-370
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    • 2017
  • This study investigated the chemical composition of headspace gas from white-flowered lotus (Nelumbo nucifera Gaertner). Volatile flavor compositions of headspace from white-flowered lotus (floral leaf, stamen, flower stalk, stem) were investigated through the solid-phase microextraction method using polydimethylsiloxane-divinylbenzene fiber. The headspace was directly transferred to a gas chromatography-mass spectrometry. Sixty-three volatile flavor constituents were detected in the headspace of lotus floral leaves, and undecanoic acid (7.81%) was the most abundant component. Fifty-three volatile flavor constituents were detected in the headspace of lotus stamina, and isobutylidene phthalide (7.94%) was the most abundant component. Forty-four volatile flavor constituents were detected in the headspace of lotus flower stalks, and 3-butyl dihydrophthalide (11.23%) was the most abundant component. Fifty-nine volatile flavor constituents were detected in the headspace of lotus stems, and ligustilide (16.15%) was the most abundant component. The content of phthalides was higher in the headspace of flower stalks and stems, while alcohols and acids were the predominant compounds in lotus floral leaves.

Evaluation of soybean oil rancidity by pentanal and hexanal determination (Pentanal과 hexanal 측정에 의한 대두유의 산패도 측정)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.149-153
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    • 1991
  • Several commercial soybean oils were stored at $20^{\circ}C,\;40^{\circ}C$ and $60^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$, The pentanal and hexanal separated were identified by gas chromatography and gas chromatography-mass spectrometric method. The results showed that the contents of pentanal and hexanal were linearly increased during storage for 100 days. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. A similar linear relationship was also obtained for acid and peroxide value with sensory data. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of soybean oil.

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Dynamic Headspace Analysis of Volatile Constituents of Swiss Cheese Whey Protein Concentrate

  • Ha, E.Y.W.;Lee, S.J.;Jung, E.J.;Lee. Y.B.;Morr, C.V.
    • Preventive Nutrition and Food Science
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    • v.7 no.3
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    • pp.299-304
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    • 2002
  • Volatile flavor compounds in the headspace of swiss cheese whey protein concentrate (WPC) were analyzed by dynamic headspace analyzer, gas chromatography, and mass spectrometer. Sixty one compounds were detected from the headspace of dry WPC and 23 compounds from the headspace of an aqueous solution of WPC. The major components were propanol, hexanal, 2-butanone, 2-pentanone, 2,3-butanedion, 2-propanol, acetic acid, dimethyl disulfide and benzothiazole. An external dynamic headspace sampler, devised for this study, effectively collected volatiles from the headspace of dry WPC and aqueous WPC solutions.

Effect of Heat Treatment on the Hexanal Content of Peanut Milk (열처리가 땅콩유중의 Hexanal 함량에 미치는 영향)

  • Lee, Chan
    • Korean Journal of Food Science and Technology
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    • v.29 no.6
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    • pp.1319-1321
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    • 1997
  • The effect of cooking peanut kernels before grinding on the hexanal content of peanut milk was investigated. Hexanal which is thought to be one of the major compounds contributing to the beany flavor of peanut milk, was quantified using a simplified headspace gas chromatographic method. Four cooking times (0, 10, 20 and 30 min) were evaluated. The concentration of hexanal in peanut milk was one-third by cooking peanut kernels for 10 min or longer. Protein content of peanut milk gradually decreased by heat treatments.

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The Study on the Measurement of Formaldehyde in Hair by HS-GC-MS (헤드스페이스-가스크로마토그래피-질량분석법에 의한 체모 중 포름알데하이드 측정법 연구)

  • Shin Ho-Sang;Ahn Hye-Sil
    • Journal of Environmental Health Sciences
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    • v.32 no.1 s.88
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    • pp.67-70
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    • 2006
  • A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

Integration of Headspace Solid Phase Micro-Extraction with Gas Chromatography for Quantitative Analysis of Formaldehyde

  • Lo, Kong Mun;Yung, Yen Li
    • Bulletin of the Korean Chemical Society
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    • v.34 no.1
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    • pp.139-142
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    • 2013
  • A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

Extraction Methods of Organic Components from Rubber Composites and Analysis of the Extract Using Gas Chromatography/Mass Spectrometry

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.54 no.3
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    • pp.188-200
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    • 2019
  • Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.

Determination of Volatile Organic Compounds (VOCs) in Drinking Water using Solid Phase Microextraction (SPME) (SPME를 이용한 수용액중의 휘발성 유기화합물 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.277-281
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    • 2000
  • The solid phase microextrction (SPME) fiber which contains $100{\mu}m$ polydimethyl siloxane of a stationary phase was used for the analysis of volatile organic compounds contained in aqueous solution. sixteen volatile organic compounds, which were spiked in blank water and extracted by the headspace SPME techique, were analyzed by gas chromatography/mass spectrometry (GC/MS). Analytical results showed that the percent of average recoveries and relative standard deviations were 97% and 4.7%, respectively. The value of detection limit was ranged from 0.01 to $0.5{\mu}g/l$. These results are more accurate than those obtained by the other methods such as purge and trap and headspace methods.

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Determination of MTBE, TBA and BTEX in Soil by Headspace Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1693-1698
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    • 2012
  • A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.