• Title/Summary/Keyword: Microextraction

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Volatile Component of Pine Needles from Pinus densiflora S. using Solid Phase Microextraction-Ges Chromatography-Mass Spectrometry

  • Lee Jae-Gon;Lee Chang-Gook;Back Shin;Jang Hee-Jin;Kwag Jae-Jin;Lee Gae-Ho
    • The Korean Journal of Food And Nutrition
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    • v.18 no.4
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    • pp.373-379
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    • 2005
  • The volatile components of Pinus densiflora needles were studied by gas chromatography-mass spectrometry(GC-MS), using seven kinds of solid phase microextraction (SPME) fibers, seven in SPME fibers: 100 ${\mu}m$ PDMS, 65 ${\mu}m$ PDMS/DVB, 65 ${\mu}m$ SF-PDMS/DVB, 85 ${\mu}m$ PA, 75 ${\mu}m$ CAR/PDMS, 65 ${\mu}m$ CW/DVB and 50/30 ${\mu}m$ DVB/CAR/PDMS fibers. A total of 40 components were identified by using the seven different SPME fibers. The identified components were classified, according to their functionalities, as follows: 26 hydro-carbons, 7 alcohols, 4 carbonyl compounds, and 3 esters. The major volatile components of Pinus densiflora needles identified by these SPME fibers were $\alpha$-pinene ($1.7\~21.7\;{\mu}g/g$), $\beta$-myrcene ($2.0\~20.1\;{\mu}g/g$), $\beta$-phel-landrene ($4.6\~22.8\;{\mu}g/g$), $\beta$-caryophyllene ($6.7\~26.0\;{\mu}g/g$) germacrene D ($1.1\~11.9\;{\mu}g/g$). In the comparison of the seven SPME fibers, PDMS appeared to be the most suitable fiber for the analysis of hydrocarbon compounds and CAR/DPMS, PDMS/DVB, CW/VB and DVB/CAR/PDMS are shown to be optimal for analysis of the alcohols and carbonyl compounds.

Analysis of caffeine in aqueous sample by hollow fiber-liquid microextraction (HF-LPME) (HF-LPME를 이용한 수용액 시료중의 카페인 분석)

  • In, Chi-Yeon;Kim, Taek-Jae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.21 no.2
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    • pp.84-92
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    • 2008
  • A method for the determination of trace amount of caffeine in urine and various drink samples using hollow fiber-liquid phase microextraction (HF-LPME) and capillary gas chromatograph/nitrogen phosphorus detector (GC/NPD) has been established. HF-LPME method has been optimized with respect to several experimental parameters including the effects of the hollow fiber length, extraction solvent, stirring mode, pH and salt concentration for the determination of caffeine from aqueous samples. The correlation coefficient of calibration curve for caffeine was 0.9994. The average recovery was 102%(n=3). The established method is feasible for the determination of trace amounts of caffeine in several aqueous sample. The limit of detection (LOD) and the limit of quantitation (LOQ) have been found to be 2.5 and 10 ng/mL, respectively. The established HF-LPME method for the analysis of caffeine from aqueous sample can be used for the determination of biological, food and environmental samples.

Volatile Aroma Compounds and Their Characteristics of Labiatae by Solid-Phase Microextraction (SPME) (Solid-Phase Microextraction (SPME)에 의한 꿀풀과 약초의 향기성분과 그 특성)

  • Song, Yong-Eun;Ku, Chang-Sub;Mun, Sung-Phil;Ryu, Ji-Sung;Kim, Dae-Hyang;Choi, Joung-Sik;Choi, Yeong-Geun
    • Korean Journal of Medicinal Crop Science
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    • v.10 no.2
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    • pp.120-125
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    • 2002
  • This study was carried out to find the possibility of use of Solid Phase Microextraction (SPME) for extracting the volatile aroma compounds in the five aromatic plants (Agastache rugosa O. Kuntze, Mentha arvensis Linne, Thymus quinquecostatus Celakovsky, Elsholtzia splendens Nakai, Schizonepta tenuifolia Briquet) belongs to the Labiatae. In the result of the analysis, the volatile aroma compounds were mainly composed monoterpene alcohol (linanol, menthol, ${\alpha}-terpineol$, borneol), monoterpene ketone (limonene, menthone) and sesquiterpene (trans-caryophyllene,${\delta}-cadinene)$. The volatile aroma compounds of Agastache rugosa O. Kuntze and Mentha arvensis Linne were extracted by SPME more identified than the SDE. However, Schizonepta tenuifolia Briquet more identified by the SDE and in Elsholtzia splendens Nakai similar to the SDE. Especially, the SPME showed the sesquiterpene contents was more than the SDE. The major volatile aroma compounds were difference but the composition of those between the SPME and the SDE showed no difference. Within the results, the SPME showed the most convenient and a rapid extraction method to analysis of the volatile aroma compounds.

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.