• Title/Summary/Keyword: Solid-phase microextraction

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Comparison of Flavor Compounds in Steamed- and Nonsteamed-Roasted Polygonatum odoratum Roots by Solid-Phase Microextraction (Solid-Phase Microextraction(SPME)을 이용한 둥굴레차의 증자 여부에 따른 향기성분 특성 비교)

  • Park, Nan-Young;Seo, Ji-Hyung;Kim, Young-Hoi;Kwon, Joong-Ho
    • Korean Journal of Food Science and Technology
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    • v.32 no.3
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    • pp.507-512
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    • 2000
  • The headspace flavors of roasted tea, prepared with steamed and nonsteamed polygonatum roots, were absorbed in solid-phase microextraction(SPME) fiber coated with $65\;{\mu}m$ of carbowax/divinylbenzene(CW/DVB) and analysed by GC-MS. The absorption conditions of SPME fiber for equilibrated headspace were selected as $60^{\circ}C$ and 30 min. In a comparison for both samples roasted at $130^{\circ}C$ for 15 min, gas chromatograms showed a similar pattern in overall profiles between steamed and nonsteamed samples before roasting, but some differences were observed in peak characteristics. From 40 separated peaks, 25 compounds were identified with both GC-MS and retention time comparison. The pyrazines including 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, 2,5-dimethyl-4-hydroxy-3(2H)-furanone, 2-acetyl-1-pyrroline, etc. were higher in their contents in nonsteamed-roasted sample than steamed-roasted one. In particular, steamed-roasted polygonatum showed higher contents of acetic acid(8.17%) and hexanoic acid(5.43%) than the corresponding compounds of nonsteamed-roasted one, 2.40% and 2.00%.

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Comparison of Solid Phase Microextraction-Gas Chromatograph/Pulsed Flame Photometric Detector (SPME-GC/PFPD) and Static Headspace-Gas Chromatograph/Pulsed Flame Photometric Detector (SH-GC/PEPD) for the Analysis of Sulfur-Containing Compounds (Solid phase microextraction-gas chromatograph/pulsed flame photometric detector(SPME-GC/PFPD)와 static headspace-gas chromatograph/pulsed flame photometric detector(SH-GC/PEPD)를 이용한 황 함유 화합물들의 분석 방법 비교)

  • Yang, Ji-Yeon;Kim, Young-Suk
    • Korean Journal of Food Science and Technology
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    • v.37 no.5
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    • pp.695-701
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    • 2005
  • Efficient method was established for analysis of sulfur-containing compounds, including dimethyl disulfide, dimethyl trisulfide, 3-methyl thiophene, allyl mercaptan, 2-methyl-3-furanthiol, and methional. Sulfur-containing compounds were extracted through solid phase microextraction (SPME) or static headspace extraction (SH), and quantified using gas chromatograph equipped with pulsed flame photometric detector. All sulfur compounds, except ally mercaptan, showed higher detection response when dissolved in hexane than in dichloromethane. Linear range was $10^2-10^4$. Dimethyl trisulfide showed lowest limit of detection (LOD) value of 15.2 ppt, and methional highest of 70.5 ppb. Highest extraction efficiency for sulfur-containing compounds, particularly polar and small molecular weight compounds, was observed in 75mm carboxen/polydimethylsiloxane fiber, followed by 65mm polydimethylsiloxane/divinylbenzene and 100mm polydimethylsiloxane. Compared to SPME, less sulfur-containing compounds could be analyzed by SH, mainly due to its low extraction efficiency, although lower amount of artifacts were formed during sample preparation.

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.

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

  • Kim, Jong-Hun;Lee, Kyung-Min
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.237-245
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    • 2007
  • The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

Liquid-phase Microextraction Pretreatment Techniques for Analysis of Chemical Warfare Agents and Their Degradation Byproducts in Environmental Aqueous Samples (환경샘플 내 화학작용제 및 분해물질 분석을 위한 Liquid Phase Microextraction (LPME) 전처리 기법)

  • Kim, Dongwook;Chung, Wooyoung;Kye, Youngsik
    • Applied Chemistry for Engineering
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    • v.26 no.1
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    • pp.17-22
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    • 2015
  • International interests in chemical warfare agents (CWAs) have been increased recently because of the use of sarin (GB) in Syrian civil war which caused around 1,300 casualties in 2013. After exposing to natural environments, CWAs undergo hydrolysis or photodegrade to non-toxic degradation byproducts. Generally, CWAs and their degradation byproducts are present at very low concentration (e.g. several ppb), thus pretreatment processes including separation, extraction and concentration are required prior to any analyses. Liquid-liquid extraction and solid-phase extraction (SPE) are common techniques to pretreat environmental samples. Recently, a novel pretreatment method, liquid phase miecoextraction (LPME), has been applied to CWAs analysis, which could reduce amounts of solvent used but promote analytical efficiencies. Fundamental backgrounds of LPME and its application to CWAs analysis were reviewed.

Comparisons of Volatile Compounds Extracted from Pinus densiflora by Headspace Analysis (Headspace법에 의한 솔향의 분석)

  • 이미정;정은주;이신조;조지은;이양봉;조현종;윤정로
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.1
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    • pp.26-31
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    • 2002
  • Volatile compounds from three parts of needles, sprouts and twigs in Pinus densiflora were extracted by solid phase microextraction (SPME) and dynamic headspace analysis (DHA). separated by gas chromatography, and identified by using mass selective detecter and Kovat's retention index. The amounts of monoterpenes isolated by SPME and DHA were 66.7% and 14.3% in needles, 90.6% and 0.7% in sprouts, and 90.6% and 1.2% in twings, respectively. The amounts of sesquiterpenes detected only by SPME were 25.8% in needles, 4.4% in twings and 1.5% in sprouts. And the amounts of oxygenated terpenes isolated by SPME and DHA were 4.7% and 79.0% in sprouts, 3.7% and 70.4% in twigs, and 1.0% and 50.7% in needles, respectively. The kinds of volatile compounds isolated by SPME were similar to those by solvent extraction, but the number of compounds identified to hate a boiling point below 5$0^{\circ}C$ by UHA was larger than that of SPME.

The Global Volatile Signature of Veal via Solid-phase Microextraction and Gas Chromatography-mass Spectrometry

  • Wei, Jinmei;Wan, Kun;Luo, Yuzhu;Zhang, Li
    • Food Science of Animal Resources
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    • v.34 no.5
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    • pp.700-708
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    • 2014
  • The volatile composition of veal has yet to be reported and is one of the important factors determining meat character and quality. To identify the most important aroma compounds in veal from Holstein bull calves fed one of three diets, samples were subjected to solid-phase microextraction (SPME) combined with gas chromatography-quadrupole mass spectrometry (GC-MS). Most of the important odorants were aldehydes and alcohols. For group A (veal calves fed entirely on milk for 90 d before slaughter), the most abundant compound class was the aldehydes (52.231%), while that was alcohols (26.260%) in group C (veal calves fed starter diet for at least 60 d before slaughter). In both classes the absolute percentages of the volatile compounds in veal were different indicating that the veal diet significantly (p<0.05) affected headspace volatile composition in veal as determined by principal component analysis (PCA). Twenty three volatile compounds showed significance by using a partial least-squared discriminate analysis (PLS-DA) (VIP>1). The establishment of the global volatile signature of veal may be a useful tool to define the beef diet that improves the organoleptic characteristics of the meat and consequently impacts both its taste and economic value.

Analysis of Haloacetonitriles in Drinking Water Using Headspace-SPME Technique with GC-MS (Handspace Solid Phase Microextraction 방법에 의한 HANs 분석에 관한 연구)

  • Cho, Deok-Hee
    • Journal of Korean Society of Water and Wastewater
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    • v.18 no.5
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    • pp.628-637
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    • 2004
  • In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of disinfection by-products (DBPs) such as haloacetonitriles (HANs), trihalomethanes (THMs), haloacetic acids (HAAs). In this study, headspace-solid phase microextraction (HS- SPME) technique was applied for the analysis of HANs in drinking water. The effects of experimental parameters such as selection of SPME fiber, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and detection limits were also evaluated. The $50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were the optimal experimental conditions for the analysis of HANs. The correlation coefficients ($r^2$) for HANs was 0.9979~0.9991, respectively. The relative standard deviations (%RSD) for HANs was 2.3~7.6%, respectively. Detection limits (LDs) for HANs was $0.01{\sim}0.5{\mu}g/L$, respectively.

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
    • Analytical Science and Technology
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    • v.30 no.2
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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.