• Title/Summary/Keyword: headspace GC

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The Analysis of Airborne Trimethylamine Using a Headspace (HS)-SPME Method (헤드스페이스-SPME 방법을 이용한 트리메틸아민의 분석방법 연구)

  • Ahn, Ji-Won;Kim, Ki-Hyun
    • Journal of Korean Society for Atmospheric Environment
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    • v.24 no.3
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    • pp.357-366
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    • 2008
  • In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

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 $mL^{-1}$.

Determination of Aroma Components in Pinus densiflora (Pine Needles) Studied by Using Different Extraction Methods (추출방법에 따른 솔잎의 휘발성 성분 조성 비교)

  • Lee Jae-Gon;Lee Chang-Gook;Baek Shin;Kwon Young-Ju;Jang Hee-Jin;Kwag Jae-Jin;Rhee Moon-Soo;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.19 no.2
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    • pp.161-168
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    • 2006
  • The efficiency of six different extraction methods for the analysis of aroma components from pine needle(P. densiflora) was compared by gas chromatography-mass selective detector(GC-MSD). The six methods were dynamic headspace(DHS), reduced pressure headspace(RPHS), solid-phase microextraction(SPME), simultaneous distillation-extraction(SDE), supercritical fluid extraction(SFE) and pyrolysis distillation extraction(PDE). A total of 65 compounds were identified by using the six different extraction methods. These compounds are classified into six categories in terms of chemical functionality: 25 hydrocarbons, 16 alcohols, 9 carbonyls, 6 esters, 7 acids, and 2 ethers. The aroma compounds having low boiling point were more abundant in DHS, RPHS, and SPME extracts. On the other hand, the aroma compounds having high boiling point were more abundants in SDE, SFE and PDE extracts. The acid compounds were extracted by heat-based extraction methods such as SDE, SFE, PDE, but not by DHS, RPHS and SPME, which used neither solvent nor heat. The oxygenated terpens, hexanal, hexanol, and hexadienal were more abundant in DHS and RPHS extracts, compared with the other methods.

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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Determination of geosmin and 2-MIB in Nakdong River using headspace solid phase microextraction and GC-MS (HS-SPME-GC/MS를 이용한 낙동강 수계 하천수 중 조류기원성 냄새물질 분석)

  • Lee, Injung;Lee, Kyoung-Lak;Lim, Tae-Hyo;Park, Jeong-Ja;Cheon, Seuk
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.326-332
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    • 2013
  • Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

Development of an Analytical Method for Chloropicrin Determination in Hulled Rice by GC-ECD and GC-MS (GC-ECD 및 GC-MS를 이용한 현미 중 chloropicrin의 잔류시험법 개발)

  • Do, Jung-Ah;Choi, Jeong-Heui;Park, Hyejin;Park, Yong-Chun;Yoon, Hae-Jung;Choi, Dongmi;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.28 no.3
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    • pp.222-226
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    • 2013
  • A simple and sensitive analytical method was developed using gas chromatograph with electron capture detector (GC-ECD) and gas chromatograph-mass spectrometer (GC-MS) for determination and identification of chloropicrin. Because of small molecular weight and high volatile properties of chloropicrin, analytical method was developed utilizing headspace extraction and direct injection to the GC. The developed method was validated using hulled rice sample spiked with chloropicrin at different concentration levels, 0.1 and 0.5 mg/kg. Average recoveries of chloropicrin (using each concentration three replicates) ranged 77.7~79.3% with relative standard deviations less than 10% and calibration solutions concentration in the range $0.005{\sim}0.5{\mu}g/mL$, and limit of detection (LOD) and limit of quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The result showed that developed analytical methods was successfully applied to detect a small amount of chloropicrin in hulled rice.

Isolation of Volatile Allelochemicals from Leaves of Perilla frutescens and Artemisia asiatica (들깨(Perilla frutescens)와 쑥(Artemisia asiatics)잎으로부터 휘발성 타감 작용 성분의 분리)

  • Lim, Sun-Uk;Seo, Young-Ho;Lee, Young-Guen;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.37 no.2
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    • pp.115-123
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    • 1994
  • Allelopathic activity of the volatiles from leaves of Perilla frutescens an Artemisia asiatica was determined on the basis of bioassay, which tested germination and seedling growth of radish, rice, mung bean and lettuce. Seedling growth was more inhibited by phytotoxic volatiles than germination. Volatile components collected by headspace cold trapping-Tenax GC adsorption were analyzed by GC-MS. Fifteen volatile components in P. frutescens and 15 components in A. asiatica were identified. By steam distillation-extraction, 4 flavor components in P. frutescens and 10 components in A. asiatica were identified. The inhibitory activity of the fractions, obtained by steam distillation-extraction, was determined by virtue of bioassay on radish. Volatile allelochemicals of the most active fraction, neutral fraction, isolated from P. frutescens contained 9 components. In A. asiatica, 24 volatile allelochemicals were identified.

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Studies on the Free and Bound Aroma Compounds in Green and Fermented Teas (녹차와 후발효차의 유리형 및 결합형 향기성분에 대한 연구)

  • Lee, Hye-Jin;Park, Seung-Kook
    • Korean Journal of Food Science and Technology
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    • v.43 no.4
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    • pp.407-412
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    • 2011
  • Free and bound aroma compounds in green and fermented teas treated with microbial-fermentation were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. Aldehydes and ketones in green tea decreased during microbial fermentation, whereas linalool and geraniol increased in the fermented tea. After enzyme treatment, (Z)-3-hexen-1-ol increased significantly following enzymatic hydrolysis of both green and fermented teas. In addition, benzaldehyde, 3-hexenyl acetate, and geraniol also increased in green tea with enzyme treatment. Bound aroma compounds in the green and fermented teas increased at different levels of added enzyme. We demonstrated the enhancement of both green and fermented teas by enzyme treatment, which can lead to improvement in the flavor qualities of green and fermented teas.

Volatile Analysis of Commercial Korean Black Raspberry Wines (Bokbunjaju) Using Headspace Solid-phase Microextraction (Headspace Solid-phase Microextraction을 이용한 시판 복분자주의 휘발성분 분석)

  • Lee, Seung-Joo
    • Korean Journal of Food Science and Technology
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    • v.46 no.4
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    • pp.425-431
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    • 2014
  • In this study, the volatile compounds in 24 commercial Korean black raspberry wines were isolated by headspace solid-phase microextraction and analyzed by gas chromatography-mass spectrometry (GC-MS). A total of 43 volatile components, including 15 esters, 12 terpenes, 7 alcohols, 4 acids, 3 ketones, and 2 aldehydes, were identified. Ethyl esters and alcohols such as ethyl acetate, ethyl octanoate, isoamyl alcohol, and phenethyl alcohol were the most represented groups among the quantified volatiles. In particular, various terpenes such as DL-limonene, linalool, alpha-terpineol, and myrtenol were identified. The differences in volatile components among the 24 black raspberry wines and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 43.9% of the total variation across the samples. No apparent sample groupings were observed according to manufacturing locations. The samples KU, BH, SR, and MO showed higher overall levels in the concentrations of terpenes originating from black raspberry, while other samples such as BB and HB, showed higher in ethyl ester and alcohol contents produced by yeast fermentation, respectively.

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.