• 제목/요약/키워드: headspace-gas chromatography

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SPME-GC-MS를 이용한 담배와 관련된 향료의 분석 (Analysis of Flavor-related Compounds from Tobacco using SPME-GC-MS)

  • 박교범;이석근
    • 분석과학
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    • 제14권2호
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    • pp.109-114
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    • 2001
  • 담배에 포함된 향료 성분을 headspace solid phase microextraction(SPME)를 이용하여 gas chromatography-mass spectrometry(GC-MS)의 selected ion monitoring(SIM)방법으로 분석하였다. 본 연구에서 사용한 담배향과 관련된 성분은 estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methylisoeugenol 및 myristicin 등 11종이며 분석결과 모든 담배에서 한가지 또는 그 이상의 담배향 성분을 $0.001-1.3{\mu}g/g$ 검출할 수 있었으며 회수율은 89.1-102.9%로 나타났고 상대표준편차는 2.6-25.2%를 얻었다.

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Determination of volatile compounds by headspace-solid phase microextraction - gas chromatography / mass spectrometry: Quality evaluation of Fuji apple

  • Lee, Yun-Yeol;Jeong, Moon-Cheol;Jang, Hae Won
    • 분석과학
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    • 제30권2호
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    • pp.68-74
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    • 2017
  • The volatile components in 'Fuji' apple were effectively determined by a headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 48 volatile components were identified and tentatively characterized based on National Institute of Standards and Technology (NIST) MS spectra library and the Kovats GC retention index I (RI). The harvested Fuji apples were divided into two groups: 1-methylcyclopropene (1-MCP) treated and non-treated (control) samples for finding important indicators between two groups. The major volatile components of both apples were 2-methylbutyl acetate, hexyl acetate, butyl 2-methylbutanoate, hexyl butanoate, hexyl 2-methylbutanoate, hexyl hexanoate and farnesene. No significant differences of these major compounds between 1-MCP treated and non-treated apples were observed during 1 month storage. Interestingly, the amount of off-flavors, including 1-butanol and butyl butanoate, in 1-MCP treated apples decreased over 5 months, and then increased after 7 months. However, non-treated apples did not show significant changes for off-flavors during 7 month storage (p<0.05). The non-treated apples also contained the higher levels of two off-flavors than 1-MCP treated apples. These two compounds, 1-butanol and butyl butanoate, can be used as quality indicators for the quality evaluation of Fuji apple.

Development of Analytical Technology Using the HS-SPME-GC/FID for Monitoring Aromatic Solvents in Urine

  • Lee, Mi-Young;Chung, Yun Kyung;Shin, Kyong-Sok
    • Mass Spectrometry Letters
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    • 제4권1호
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    • pp.18-20
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    • 2013
  • Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

Correlation Between Total Mercury and Methyl Mercury-In Whole Blood of South Korean

  • Jung, Seon A;Chung, Dayoung;On, Jiwon;Moon, Myeong Hee;Lee, Jeongae;Pyo, Heesoo
    • Bulletin of the Korean Chemical Society
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    • 제34권4호
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    • pp.1101-1107
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    • 2013
  • In this study, total mercury and methyl mercury in whole blood of Korean was analyzed so as to investigate the correlation between total mercury (T-Hg) and methyl mercury (Me-Hg). 4000 whole blood samples were divided in four groups, according to T-Hg concentration in percentile: group I (p25-p50), group II (p50-p75), group III (p75-p95) and group IV (p95-p100). 100 samples were randomly selected from the each group, and Me-Hg concentration was measured. T-Hg concentration in whole blood was analyzed using a Direct Mercury Analyzer-80 and obtained limit of detection (LOD) was $0.2{\mu}gL^{-1}$. Me-Hg concentration was analyzed with ethylate derivatization using headspace-gas chromatography-mass spectrometry, and obtained LOD of methyl mercury was $0.5{\mu}gL^{-1}$. The geometric means of T-Hg and Me-Hg were $6.35{\mu}gL^{-1}$ and $4.44{\mu}gL^{-1}$, respectively, and 71.91% of T-Hg was presented as Me-Hg.

Volatile Metabolic Markers for Monitoring Pectobacterium carotovorum subsp. carotovorum Using Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

  • Yang, Ji-Su;Lee, Hae-Won;Song, Hyeyeon;Ha, Ji-Hyoung
    • Journal of Microbiology and Biotechnology
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    • 제31권1호
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    • pp.70-78
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    • 2021
  • Identifying the extracellular metabolites of microorganisms in fresh vegetables is industrially useful for assessing the quality of processed foods. Pectobacterium carotovorum subsp. carotovorum (PCC) is a plant pathogenic bacterium that causes soft rot disease in cabbages. This microbial species in plant tissues can emit specific volatile molecules with odors that are characteristic of the host cell tissues and PCC species. In this study, we used headspace solid-phase microextraction followed by gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS) to identify volatile compounds (VCs) in PCC-inoculated cabbage at different storage temperatures. HS-SPME-GC-MS allowed for recognition of extracellular metabolites in PCC-infected cabbages by identifying specific volatile metabolic markers. We identified 4-ethyl-5-methylthiazole and 3-butenyl isothiocyanate as markers of fresh cabbages, whereas 2,3-butanediol and ethyl acetate were identified as markers of soft rot in PCC-infected cabbages. These analytical results demonstrate a suitable approach for establishing non-destructive plant pathogen-diagnosis techniques as alternatives to standard methods, within the framework of developing rapid and efficient analytical techniques for monitoring plant-borne bacterial pathogens. Moreover, our techniques could have promising applications in managing the freshness and quality control of cabbages.

Effects of Broth pH and Chilling Storage on the Changes in Volatile Profiles of Boiled Chicken Flesh

  • Pattarabhorn Pakaweerachat;Teerin Chysirichote
    • 한국축산식품학회지
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    • 제44권5호
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    • pp.1096-1107
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    • 2024
  • This study investigated the changes in volatile compounds in chicken flesh after boiling at various pHs (6.0-9.0) and after chilling storage (4.0±1.0℃) for 7 d. The volatile compounds were assessed qualitatively and quantitatively by using a headspace gas chromatography-mass spectrometry analysis. Twenty-one volatile compounds were discovered and categorized as amine, aldehyde, alcohol, ketone, acid, and furan. One type of amine, (2-aziridinylethyl) amine, was the most prevalent volatile component, followed by aldehyde, ketone, aldehyde, acid, ester, and furan. The results showed that the quantity and quality of the volatile compounds were influenced by a pH of the boiling medium. Additionally, the types and volatile profiles of the chicken were altered during chilling. In particular, in the chicken that was boiled at a pH of 8.0, the hexanal (an aldehyde) content increased the most after 7 d of chilling. Moreover, various alcohols formed after the 7 d of chilling of the chicken that was boiled at pHs of 8.0 and 9.0. Because of the oxidation and degradation of fat and proteins, the most altering volatile compounds were the reducing amines and the increasing aldehydes.

향끽미종 잎담배 성분조성에 관한 연구 II. 헤드스페이스 휘발성 유기성분의 특성 조사 (Composition Studies on the Aromatic Tobacco Varieties (Nicotiana tabacum L. ) : II. Characteristics of Headspace Vapors)

  • 김경례;이운철
    • 한국연초학회지
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    • 제3권1호
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    • pp.1-10
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    • 1981
  • 5가지 향끽미종 잎담배의 헤드스페이스 휘발성 성분들을 중합체 흡착방법 및 고성능 유리 캐피러리 가스 크로마토그라피로 분석하였다. 얻어진 가스 크로마토그라피의 프로파일을 비교한 결과 각 담배 시료는 독특한 방향성분의 조성을 보여주며 주요성분의 정량적인 차이가 현저함이 확인되었다.

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

  • 김종훈;이경민
    • 분석과학
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    • 제20권3호
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    • pp.237-245
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    • 2007
  • 현재 시중에서 판매되고 있는 비타민드링크 제품 중 20개사 31개 제품의 벤젠 함량을 headspace-solid phase microextraction(HS-SPME)법을 이용하여 GC/MS-SIM으로 분석을 하였다. SPME fiber는 $100{\mu}m$ PDMS를 사용하였다. 또한 정량방법은 표준물첨가법을 사용하였으며 40 mL vial에 용액 25 mL를 취하고 그 안에 자석젓개를 넣어 1200 rpm에서 교반시키고 4분 동안 흡착시킨 후 1분 동안 GC에서 탈착시켜 표준검량곡선을 작성하였다. 이 때 검량곡선의 상관계수 값은 0.999이상을 나타내었다. 검출한계는 시료를 분석할 때마다 산출하였는데 평균값이 0.56 ng/mL(${\pm}0.43$)이었으며 회귀식이 존재하는 농도의 범위는 0~40 ng/mL였다. 그 결과 시료 중 벤젠의 함유량은 nd~47.35 ng/mL의 농도의 범위였다. 전체 시료 중 15개의 제품에서 벤젠이 검출되었으며 그 중 5개의 제품에서는 벤젠의 함량이 먹는 물 수질기준인 10 ng/mL를 넘는 각각 16.99 ng/mL, 35.14 ng/mL, 16.03 ng/mL, 47.35 ng/mL, 14.28 ng/mL가 검출되었다.

헤드스페이스 고체상미량추출(Solid-Phase Microextraction)을 이용한 시판 일본소주의 휘발성 향기성분 분석 (Volatile Component Analysis of Commercial Japanese Distilled Liquors (Shochu) by Headspace Solid-Phase Microextraction)

  • 신광진;이승주
    • 한국식품과학회지
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    • 제47권5호
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    • pp.567-573
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    • 2015
  • 일본 증류식 소주인 본격소주 9종을 수거하여 시료의 휘발성 향기성분을 헤드스페이스-고체상미량추출법에 의해 추출한 후, 가스크로마토그래피-질량분석기를 이용하여 분석하였다. 총 76개의 성분이 동정되었고, 화학적 특성에 따라 분류하면 에스터 48종, 알코올 13종, 기타 15종의 성분이 동정되었다. 에스터와 알코올이 주요한 성분으로 분석되었으며 아세트산아이소아밀, 폼산아이소아밀, 헥산산에틸, 옥탄산에틸, 데카노산에틸, 아이소아밀알코올, 2-페닐에탄올이 주요 성분으로 나타났다. 주성분 분석 결과 제조원료에 따라 주성분1 선상에서 대맥국 원료 본격소주의 향기패턴이 큰 차이를 보이는 것으로 나타났으며 쌀과 보리 원료에 따른 향기패턴의 차이는 크게 나타나지 않았다. 본 연구의 일본 본격소주 휘발성 향기성분 분석 결과와 국내산 증류식 소주의 주요 향기성분 분석 결과를 비교분석하면 향후 국내산 증류식 소주의 품질관리에 주요한 향기성분 파악이 가능하고 이를 통해 다양한 원재료와 제조방법에 따른 증류식 소주 제품 개발이 가능하리라 여겨진다.

Dynamic Headspace법에 의한 분획별 된장의 향기 성분 (Fractionated Volatile Flavor Components of Soybean Paste by Dynamic Headspace Method)

  • 주광지;신묘란
    • 한국식품영양과학회지
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    • 제28권2호
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    • pp.305-311
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    • 1999
  • The volatile compounds of soybean pastes(home made soondoenjang, commercial doenjang) were classified into basic, acidic and neutral fractions by dynamic headspace method. The fractionated flavor isolates were analyzed and identified by gas chromatography mass spectrometry. Each peak area of the flavor components was quantified at its ratio to the peak area of internal standard. Sixty one compounds from home made soondoenjang, and forty three compounds from commercial doenjang were identified. The different distribution of volatile compounds between the two soybean paste samples was observed. Ten pyrazines and benzothiazole were identified in the basic fraction of home made soondoenjang. On the other hand, trimethylpyrazine was the only one of nitrogen containing compounds in the commercial doenjang, which was made from soybean(28.3%), wheat(22.2%) and alcohols. The factors which influenced the levels of these identified compounds were considered to be the starting materials of soybean paste. Alcohols, esters and aldehydes in the neutral fraction of both samples were seemed to be characterisitic soybean paste flavor and showed much higher quantities than those of the basic or acidic fractions. Furfural in the commercial doenjang was the highest content (45.28ppm) among all of the compounds identified in the samples.

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