• 제목/요약/키워드: headspace-gas chromatography

검색결과 133건 처리시간 0.02초

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 $mL^{-1}$.

Headspace Volatile Compounds of Steamed Liriopis Tuber Tea Affected by Steaming Frequency

  • Park, Jin-Yong;Park, So-Hae;Lee, Heeseob;Lee, Yang-Bong
    • Preventive Nutrition and Food Science
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    • 제19권4호
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    • pp.314-320
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    • 2014
  • Flavor quality of Liriopis tuber tea that was made using a steaming process was studied by measuring changes in headspace volatile compounds. Headspace volatile compounds of the prepared samples were isolated, separated and identified by the combined system of purge & trap, automatic thermal desorber, gas chromatography, and mass selective detector. As steaming frequencies were increased, the area percent of aldehydes decreased from 32.01% to 3.39% at 1 and 9 steaming frequency times, respectively. However, furans and ketones increased from 18.67% to 33.86% and from 9.60% to 17.40% at 1 and 9 times, respectively. The savory flavor of Liriopis tuber tea was due to a decrease in aldehydes contributing a fresh flavor at the 1st steaming process and newly generated furans from nonenzymatic browning with repeated steaming frequencies. These results will provide basic information for quality control of the newly developed Liriopis tuber tea.

Headspace - GC/ECD를 이용한 수중의 미량 요오드계 트리할로메탄류 분석 (Analysis of Trace Levels of Lodinated Trihalomethanes in Water Using Headspace - GC/ECD)

  • 손희종;송미정;김경아;염훈식;최진택
    • 대한환경공학회지
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    • 제36권1호
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    • pp.35-41
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    • 2014
  • 소독부산물의 일종인 트리할로메탄류(THMs)는 정수처리 공정에서 소독제로 사용되는 염소와 수중에 잔존하는 유기물질이 반응하여 생성된다. 일반적으로 염소계 및 브롬계 THMs는 일반적인 수돗물에서 검출되기 때문에 잘 알려져 있으나, 요오드계 THMs (I-THMs)의 경우는 수중에 요오드 이온이 존재할 때 생성된다. I-THMs는 약품취를 유발하며, 또한 염소계나 브롬계 THMs에 비해 인체독성이 더 강한 것으로 알려져 있다. 현재 I-THMs 분석을 위한 공인된 분석법은 없는 실정이다. 10종의 THMs 분석을 위해 headspace 전처리장치와 GC/ECD를 이용하여 최적화된 분석법을 개발하였으며, 개발된 분석법에 의한 검출한계(LOD)와 정량한계(LOQ)는 각각 12 ng/L~56 ng/L 및 38 ng/L~178 ng/L로 나타났다. 강물, 해수 및 하수처리장 최종방류수의 matrix 영향을 평가하였으며, 본 연구에서 개발된 분석법은 별도의 전처리 과정이 필요치 않아 간편하고 빠르며 자동화된 방법으로 수중에 미량으로 함유된 I-THMs 분석에 적합한 것으로 나타났다.

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

  • 김정한;김경례;김재정;오창환
    • 한국식품과학회지
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    • 제24권2호
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    • pp.171-176
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    • 1992
  • 더덕(Codonopsis lanceolata)의 휘발성 향기성분을 분석하기 위해 gas co-distillation(GCD), solvent extraction/fractionation(SLF), headspace sampling(HSS) 방법을 사용하여 향기성분을 분리농축하고 분석 비교한 결과 SEF와 HSS 방법으로 얻은 농축물들의 향이 원래의 더덕향과 가장 유사했으며 gas chromatogram들의 양상도 비슷했으나 peak들의 크기에 있어서 차이를 보였다. SEF 농축물에서는 달콤한 향을 기리고 HSS 농축물에서는 풋내를 비교적 강하게 느낄 수 있었으나 GCD 농축물의 경우 일정 증류시간이 지나면 한악취를 느낄 수 있었다. SEF와 HSS 방법은 GCD에 비해서 적은 조작 단계로 손쉽게 빠른 시간내에 분리 농축이 가능했다. 농축한 향기성분은 GC-MS와 극성이 다른 두 column을 사용한 GC-RI system을 이용하여 확인하였다. 특히 GC-RI는 isomer의 확인에 효과적이었으며 극성 FFAP column은 극성 화합물의 확인에 보다 적합했다. 35가지의 향기성분들을 동정하였는데 그중 24개의 성분들은 simultaneous distillation extraction 농축물에서는$^{(5)}$ 확인되지 않았던 향기성분들이다. 화인된 성분들중 trans-2-hexenal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, hexanol은 더덕의 풋내를, 1-octen-3-ol은 신선한 풍미를 그리고 amyl propionate를 비롯한 다수의 에스터 화합물 등은 더덕 특유의 달콤한 향에 복합적으로 작용할 것으로 추정된다.

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Volatile Compounds for Discrimination between Beef, Pork, and Their Admixture Using Solid-Phase-Microextraction-Gas Chromatography-Mass Spectrometry (SPME-GC-MS) and Chemometrics Analysis

  • Zubayed Ahamed;Jin-Kyu Seo;Jeong-Uk Eom;Han-Sul Yang
    • 한국축산식품학회지
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    • 제44권4호
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    • pp.934-950
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    • 2024
  • This study addresses the prevalent issue of meat species authentication and adulteration through a chemometrics-based approach, crucial for upholding public health and ensuring a fair marketplace. Volatile compounds were extracted and analyzed using headspace-solid-phase-microextraction-gas chromatography-mass spectrometry. Adulterated meat samples were effectively identified through principal component analysis (PCA) and partial least square-discriminant analysis (PLS-DA). Through variable importance in projection scores and a Random Forest test, 11 key compounds, including nonanal, octanal, hexadecanal, benzaldehyde, 1-octanol, hexanoic acid, heptanoic acid, octanoic acid, and 2-acetylpyrrole for beef, and hexanal and 1-octen-3-ol for pork, were robustly identified as biomarkers. These compounds exhibited a discernible trend in adulterated samples based on adulteration ratios, evident in a heatmap. Notably, lipid degradation compounds strongly influenced meat discrimination. PCA and PLS-DA yielded significant sample separation, with the first two components capturing 80% and 72.1% of total variance, respectively. This technique could be a reliable method for detecting meat adulteration in cooked meat.

Effect of Stewing Time on the Small Molecular Metabolites, Free Fatty Acids, and Volatile Flavor Compounds in Chicken Broth

  • Rong Jia;Yucai Yang;Guozhou Liao;Yuan Yang;Dahai Gu;Guiying Wang
    • 한국축산식품학회지
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    • 제44권3호
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    • pp.651-661
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    • 2024
  • Chicken broth has a taste of umami, and the stewing time has an important effect on the quality of chicken broth, but there are fewer studies on the control of the stewing time. Based on this, the study was conducted to analyze the effects of different stewing times on the sensory, small molecular metabolites, free fatty acids, and volatile flavor compounds contents in chicken broths by liquid chromatography-quadrupole/time-of-flight mass spectrometry, gas chromatography-mass spectrometry, headspace solid-phase microextraction, and gas chromatography-mass spectrometry. Eighty-nine small molecular metabolites, 15 free fatty acids, and 86 volatile flavor compounds were detected. Palmitic and stearic acids were the more abundant fatty acids, and aldehydes were the main volatile flavor compounds. The study found that chicken broth had the best sensory evaluation, the highest content of taste components, and the richest content of volatile flavor components when the stewing time was 2.5 h. This study investigated the effect of stewing time on the quality of chicken broth to provide scientific and theoretical guidance for developing and utilizing local chicken.

복합 유기혼합물체로부터 휘발성이 서로 다른 세 유기화합물 그룹의 분리 농축방법의 연구 (Isolation and Concentration of Organic Components from a Complex Matrix into Three Fractions of Different Volatilities)

  • 김경례
    • 대한화학회지
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    • 제25권1호
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    • pp.30-37
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    • 1981
  • 복합 유기혼합체로부터 휘발성이 다른 세 그룹을 분리 농축할 수 있는 간단한 소형장치가 고안되었다. 이 장치를 사용하여 휘발성이 높은 유기성분들은 테넥스지씨에 헤드스페이스 트랩핑하고 남은 시료를 유기용매로 용출하여 얻어진 용출들을 휘발성 및 비휘발성 그룹으로 분리 농축할 수 있었다. 얻어진 휘발성 성분그룹은 고성능 캐리러리 가스크로마토그래피로 분석하였고, 비휘발성 성분그룹은 고성능 액체크로마토그래피에 의해서 분석하였다. 상세한 실험방법 및 유기 혼합물질인 잎담배를 시료로 사용하여 얻어진 분석 결과가 언급되어 있다.

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D-Glucose-Glycine 계의 Maillard 반응생성물 및 그 생성기구 (Maillard Reaction Products Formed from D-Glucose-Glycine, System and Their Formation Mechanism)

  • 김선봉;박영호
    • 한국수산과학회지
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    • 제19권1호
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    • pp.45-51
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    • 1986
  • D-glucose-glycine 계를 사용하여 Maillard 반응에 의하여 생성되는 저분자 휘발성성분을 비롯하여 amide 화합물의 생성 및 그 기구를 검토하였다. 그 결과, 동정된 저분자 휘발성성분 중에서, headspace gas 중의 휘발성성분은 furan, acetone, 2-methylfuran, 2,5-dimethylfuran 2-butanone 2,3-pentanedione, diacetyl 등이었다, 이 중에서 diacetyl의 생성량이 가장 많아, 전 peak 면적의 약 $70\%$를 차지하였다. 또한, 에테르 추출물중의 주요반응생성물은 초산, furfuryl alcohol 2,5-dimethylpyrrole 2-acetylpyrrole 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one 등이었고, ethyl acetate 로 추출한 산성획분중에는 N-acetyl-glycine와 N-methylacetamide 등 2종류의 amide 화합물의 생성이 밝혀졌다. 이들 amide 화합물적 생성기구를 밝히기 위하여, Mailiard 반응초기생성물인 diacetyl 및 glyoxal을 각각 butylamine과 반응시킨 결과, Schiff 염기의 산화적 분해로 N-butylacetamide 및 N-butylformamide의 생성이 인정되었다. 따라서 N-acetylglycine 및 N-methylacetamide는 glucosylamine의 2,3-enol 화 및 ${\beta}-elimination$에 의한 탈수의 진행으로 생성된 dicarbonyl 화합물이 glycine과 반응하여 Schiff 염기를 형성하고, 이 Schiff 염기가 산화적분해를 받아서 N-acetylglycine이 생성되고, N-methylacetamide는 N-acetylglycine의 탈탄산에 의해서 생성된다고 생각한다.

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Headspace 법을 이용한 생굴 및 굴 자숙액의 감마선 조사에 의한 휘발성 냄새 성분 변화 분석 (Analysis of Volatile Flavor Compounds in Raw Oyster and Oyster Cooking Drips by Gamma Irradiation Using Headspace Method)

  • 최종일;김현주;이주운
    • KSBB Journal
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    • 제26권2호
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    • pp.177-181
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    • 2011
  • This study was conducted to investigate the effects of gamma irradiation on the change of volatile flavor compounds of raw oyster and its cooking drips using headspace methods. Major volatile flavor compounds of the raw oyster were identified as methylthiomethane and 1,5-hexadiene. When the raw oyster was irradiated at the dose of 5 kGy, 1-pentane was newly detected. On the other hand, 9 compounds including N-methoxyformaldehyde were identified as the major volatile compounds of cooking drips from oyster. Among them, N-methoxyformaldehyde contents in cooking drip was decreased by the gamma irradiation. By the gamma irradiation above 30 kGy, new heterocyclic compounds was found in oyster cooking drips. Therefore, the amount of volatile flavor compounds in the raw oyster and cooking drips were changed by gamma irradiation, and these results could be potentially used in the seasoning industry.

Headspace GC-MS Analysis of Spring Blossom Fragrance at Chungnam National University Daedeok Campus

  • Choi, Yeonwoo;Lee, Sanghyun;Kim, Young-Mi;Nguyen, Huu-Quang;Kim, Jeongkwon;Lee, Jaebeom
    • Mass Spectrometry Letters
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    • 제13권4호
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    • pp.125-132
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    • 2022
  • There are many types of spring blossoms on the Daedeok campus of Chungnam National University (CNU) at the area of 1,600,000 square meters. As an assignment for the class of Analytical Chemistry I for second-year undergraduate students, 2021, flower petals collected from various floral groups (Korean azalea, Korean forsythia, Dilatata lilac, Lilytree, Lily magnolia, and Prunus yedoensis) were analyzed using headspace extraction coupled to gas chromatography-mass spectrometry (HS-GC-MS) to study the aromatic profiles and fragrance compounds of each sample group. Various types of compounds associated with the aroma profiles were detected, including saturated alcohols and aldehydes (ethanol, 1-hexanol, and nonanal), terpenes (limonene, pinene, and ocimene), and aromatic compounds (benzyl alcohol, benzaldehyde). The different contribution of these compounds for each floral type was visualized using statistical tools and classification models based on principal component analysis with high reliability (R2 = 0.824, Q2 = 0.616). These results showed that HS-GC-MS with statistical analysis is a powerful method to characterize the volatile aromatic profile of biological specimens.