• Title/Summary/Keyword: Headspace solid-phase microextraction

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Determination of benzene, toluene, ethylbenzene and o-xylene in bottled waters by headspace solid-phase microextraction and gas chromatography/mass spectrometry (HS-SPME-GC/MS를 이용한 먹는 샘물 중 벤젠, 톨루엔, 에칠벤젠, 자일렌의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.119-126
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    • 2011
  • Abstract: The amount of benzene, toluene, ethylbenzene, and o-xylene (BTEX) in 30 kinds of bottled waters purchased from market and 9 kinds of tap waters from home were determined using headspace solid phase microextraction (HS-SPME). The sample was stirred at 1200 RPM G for 4 min using a magnetic bar with $100\;{\mu}m$ PDMS as adsorbent for BTEX. Then it was desorbed from the fiber for 1 min at room temperature. Quantitation was achieved using standard calibration method. The limit of detection was determined as benzene 0.39 (${\pm}0.04$) ng/mL, toluene 0.08 (${\pm}0.04$) ng/mL, ethylbenzene 0.04 (${\pm}0.01$) ng/mL, and o-xylene 0.05 (${\pm}0.02$) ng/mL. Benzene and o-xylene were not detected in any samples, but toluene was detected in 11 samples, and ethylbenzene was detected just in 3 samples among 30 investigated bottled waters. The concentration range of investigated materials for toluene and o-xylene were $0.24({\pm}0.09)\sim2.95\;({\pm}0.08)\;ng/mL$, $0.08({\pm}0.06)\sim0.93({\pm}0.10)\;ng/mL$, respectively.

Characteristics of Volatile Compound Adsorption from Alcoholic Model Solution onto Various Activated Carbons (알코올모델용액을 이용한 여러 종류 활성탄의 휘발성화합물 흡착특성)

  • Park, Seung-Kook;Lee, Myung-Soo;Kim, Byung-Ho;Kim, Dae-Ok
    • Food Engineering Progress
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    • v.14 no.3
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    • pp.249-255
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    • 2010
  • Ten commercial activated carbons (ACs) prepared from four different sources (bamboo, wood, peat, and coal) were evaluated for their adsorptive efficiency of six volatile compounds (isoamyl alcohol, hexanal, furfural, ethyl lactate, ethyl octanoate, 2-phenyl ethanol) which were dissolved in a 30% alcoholic model solution. These six volatile compounds are frequently found in alcoholic beverages and possibly contribute to physiological hangover due to their high concentrations. They are also generally regarded as off-flavor compounds at certain levels in alcoholic beverages such as whisky and vodka. Two hundred mL of 30% alcoholic solutions containing these six volatile compounds were treated with 0.2 g of ACs while stirring for 16 hr; the treated solutions were then measured for their adsorptive efficiencies (or removal efficiencies) by gas chromatographic analysis using two different sampling methods (direct liquid injection and headspace-solid phase microextraction). The adsorptive efficiencies of the ACs varied depending on the identity of the volatile compounds and the source material used for making the ACs. Ethyl octanoate, 2-phenyl ethanol, and hexanal were removed at high efficiencies (34-100%), whereas isoamyl alcohol, ethyl lactate, and furfural were removed at low efficiencies (5-13%). AC prepared from bamboo showed a high removal efficiency for isoamyl alcohol, aldehydes (hexanal and furfural), and 2-phenyl ethanol; these major fusel oils have been implicated as congeners responsible for alcohol hangover.

Analysis of Volatile Compounds in Leaves and Fruits of Zanthoxylum schinifolium Siebold et Zucc. & Zanthoxylum piperitum DC. by Headspace SPME (SPME법에 의한 산초나무와 초피나무 잎과 열매의 향기성분 분석)

  • Cho, Min-Gu;Kim, Hui;Chae, Young-Am
    • Korean Journal of Medicinal Crop Science
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    • v.11 no.1
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    • pp.40-45
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    • 2003
  • Volatile components in the leaves and fruits of Z. schinjfolium and Z. piperitum were analyzed by Headspace SPME(Solid phase Microextraction). Fifty two and 48 components in the leaves and fruits, repectively, were identified in Z. schinifolium. (E)-2-hexenal, ${\alpha}-pinene$, (Z)-ocimene+limonene, estragole, germacrene-d were detected at common components in the leaves and estragole in the fruits of Z. schinjfolium. Regardless of collection sites hexanal, (Z)-3-hexenol, (E)-2-hexenal, n-hexanol were appeared in the leaves while undecanone in the fruits. Thirty and 27 components in the leaves and fruits, respectively, were identified in Z. piperitum. ${\alpha}-pinene,\;{\beta}-phellandrene$, 1,8-cineole, citronellal and myrcene, (Z)-ocimene+limonene, ${\beta}-phellandrene$ were appeared as common components in the leaves and fruits collected from Baeck-yang-sa and Nae-jang-sa. (Z)-3-hexenol, (E)-2-hexenal, ${\alpha}-pinene\;myrcene\;and\;{\beta}-phellandrene$, citronellal, geranyl acetate were major components in the leaves and fruits from Tong-do-sa.

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.

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.

Competitive Extraction of Chlorinated Solvents by Headspace SPME GC/FID (Headspace SPME GC/FID를 이용한 Chlorinated Solvents의 경쟁적 추출효과에 관한 연구)

  • An, Sangwoo;Kim, Youngju;Chun, Sukyoung;Lee, Sijin;Park, Jaewoo;Chang, Soonwoong
    • Journal of the Korean GEO-environmental Society
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    • v.11 no.5
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    • pp.61-67
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    • 2010
  • In this study, Solid-phase microextraction (SPME) with GC/FID was studied as a possible alternative to liquid-liquid extraction for the analysis of chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). Experimental parameters affecting the SPME process (such as kind of fibers, adsorption time, desorption time, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. Experimental parameters such as CAR/PDMS, adsorption time of 20 min, desorption time of 5 min at $250^{\circ}C$, headspace volume of 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.

Impact of High Temperature on the Maillard Reaction between Ribose and Cysteine in Supercritical Carbon Dioxide

  • Xu, Honggao;He, Wenhao;Liu, Xuan;Gao, Yanxiang
    • Food Science and Biotechnology
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    • v.18 no.1
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    • pp.66-72
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    • 2009
  • An aqueous ribose-cysteine model system (initial pH 5.6) was conventionally heated to the same browning at varying temperatures ($120-180^{\circ}C$), supercritical carbon dioxide (SC-$CO_2$, 20 MPa) was also applied on the same matrices for same periods at each temperature and about 20% reduction of the absorbance at 420 nm was observed as compared with sole thermal treatment. The headspace volatiles from Maillard reaction mixtures were analyzed by solid-phase microextraction (SPME) in combination with gas chromatography and mass spectrometry (GC-MS), and predominated with sulfur containing compounds, such as thienothiophenes, polysulfur alicyclics, thiols, and disulfides. Reaction temperature exhibited complex effects on volatiles formation and those effects became further complicated by the SC-$CO_2$ treatment. The formation of noncarbonyl polysulfur heterocyclic compounds and thienothiophenes was generally favored at high temperatures. Most volatiles were inhibited in SC-$CO_2$ as compared with thermal treatment alone, however, the well-known meaty aromatic compounds, such as thiols and disulfides, were obviously enhanced.

Attraction of the Invasive Hornet, Vespa velutina nigrithorax, by using Bacillus sp. BV-1 Cultures

  • Lim, Da Jung;Lee, Jeong Eun;Lee, Jin Sil;Kim, Iksoo;Kim, In Seon
    • Korean Journal of Environmental Agriculture
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    • v.38 no.2
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    • pp.104-109
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    • 2019
  • BACKGROUND: The invasive hornet Vespa velutina nigrithorax has becomes a public concern in rural and urban South Korea. The technologies are necessary to develop a way to counter V. velutina. In an effort to develop a way to counter V. velutina, we found that a bacillus strain, named Bacillus sp. BV-1, produces volatile compounds that attract V. velutina. METHODS AND RESULTS: Field trials of V. velutina attraction were performed using plates and traps containing BV-1 cultures grown on sugar medium. When the sugar medium and sugar-grown BV-1 cultures in the plates were placed close together, V. velutina visited preferably the plates with the BV-1 cultures. Significantly more V. velutina were caught in the traps containing BV-1 cultures than in those containing only sugar medium. Headspace solid-phase microextraction coupled with GC/MS analysis of BV-1 cultures detected 2-methyl-1-propanol, 3-methyl-1-butanol, 3-methylbutanoic acid, ethyl hexanoate, 2-pheylethanol, ethyl octanoate, and ethyl decanoate as the major volatiles. CONCLUSION: BV-1 cultures were suggested as potential agents for managing V. velutina as they produce volatile compounds that attract the hornet.

Volatile Components Analysis using SPME in Traditional Aromatic Plant Resources, Zanthoxylum schinifolium Siebold et Zucc. and Z. piperitum DC (SPME법을 이용한 전통 향료 유전자원 산초 및 초피의 정유성분 분석)

  • Cho, Min-Gu;Chae, Young-Am;Song, Ji-Sook
    • Korean Journal of Medicinal Crop Science
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    • v.9 no.3
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    • pp.192-197
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    • 2001
  • This study was carried out to select proper SPME fiber for volatile component analysis in Zanthoxylum schinifolium and Z. piperitum. PDMS, PDMS/DVB and CAR/PDMS were better for single standard absorption analysis. PDMS and PDMS/DVB showed similar results in comparison between direct injection and the mixture of 24 single standards as well as the mixture of 10 single standards. PDMS and PDMS/DVB were not different each other in absorption patterns between direct injection and headspace SPME regardless of split ratio of GC injection port. However PDMS/DVB rather than PDMS was effective in absorbing the sesquiterpenes within 30-40 minutes as using the SDE extracts from Z. schinifolium and Z. piperitum.

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Evaluating the Headspace Volatolome, Primary Metabolites, and Aroma Characteristics of Koji Fermented with Bacillus amyloliquefaciens and Aspergillus oryzae

  • Seo, Han Sol;Lee, Sunmin;Singh, Digar;Park, Min Kyung;Kim, Young-Suk;Shin, Hye Won;Cho, Sun A;Lee, Choong Hwan
    • Journal of Microbiology and Biotechnology
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    • v.28 no.8
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    • pp.1260-1269
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    • 2018
  • Production of good Koji primarily depends upon the selection of substrate materials and fermentative microflora, which together influence the characteristic flavor and aroma. Herein, we performed comparative metabolomic analyses of volatile organic compounds (VOCs) and primary metabolites for Koji samples fermented individually with Bacillus amyloliquefaciens and Aspergillus oryzae. The VOCs and primary metabolites were analyzed using headspace solid phase microextraction (HS-SPME) followed by gas chromatography time-of-flight mass spectrometry (GC-TOF-MS). In particular, alcohols, ketones, and furans were mainly detected in Bacillus-fermented Koji (Bacillus Koji, BK), potentially due to the increased levels of lipid oxidation. A cheesy and rancid flavor was characteristic of Bacillus Koji, which is attributable to high content of typical 'off-flavor' compounds. Furthermore, the umami taste engendered by 2-methoxyphenol, (E,E)-2,4-decadienal, and glutamic acid was primarily detected in Bacillus Koji. Alternatively, malty flavor compounds (2-methylpropanal, 2-methylbutanal, 3-methylbutanal) and sweet flavor compounds (monosaccharides and maltol) were relatively abundant in Aspergillus-fermented Koji (Aspergillus Koji, AK). Hence, we argue that the VOC profile of Koji is largely determined by the rational choice of inocula, which modifies the primary metabolomes in Koji substrates, potentially shaping its volatolome as well as the aroma characteristics.