• Title/Summary/Keyword: GC-SPME

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Analysis of Volatile Organic Compounds in Kinnchi Absorbed in SPME by GC-AED and GC-MSD (SPME로 포집한 김치 휘발성분의 GC-AED및 GC-MSD에 의한 동정)

  • 하재호
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.31 no.3
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    • pp.543-545
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    • 2002
  • The volatile compounds in kimchi adsorbed with solid phase microextraction (SPM) were analyzed by using a gas chromatograph-atomic emission detector (GC-AED) and a gas chromatograph-mass spectrometer (GC-MSD). The volatile compounds were effectively adsorbed in SPME. Twenty five compounds such as dimethyl-sulfide were identified by GC-MSD and some of these were further confirmed to contain a sulfur and a nitrogen by GC-AED.

Volatile Components in Persimmon Vinegars by Solid-Phase Microextraction (Solid-Phase Microextraction(SPME)을 이용한 감식초의 휘발성 성분 분석)

  • Seo, Ji-Hyung;Park, Nan-Young;Jeong, Yong-Jin
    • Korean Journal of Food Science and Technology
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    • v.33 no.1
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    • pp.153-156
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    • 2001
  • Traditional static headspace and headspace solid-phase microextraction(SPME) techniques were compared for their effectiveness in the extraction of volatile flavor compounds from the headspace of persimmon vinegar. The adsorption condition of SPME fiber for equilibrated headspace vapor was selected as $80^{\circ}C$ and 20 min. Total FID response for volatiles of persimmon vinegar was exactly higher such as total peak area $18.18{\times}10^6$ in SPMEGC technique than total peak area $1.35{\times}10^6$ in static headspace-GC. The major volatiles in persimmon vinegar were acetic acid, ethyl acetate, 3-hydroxy-2-butanone, ethanol, phenethyl alcohol. From static headspace-GC technique, 3 acids, 3 aldehydes, 5 alcohols, 9 esters and 1 ketone were identified. From SPME-GC technique, total 34 compounds including 6 acids, 7 aldehydes, 6 alcohols, 9 esters, 2 hydrocarbones, 1 ketone, 3 others were detected. Also the ratio for benzaldehyde, phenethylacetate and phenethylalcohol were higher in SPME-GC.

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Correlation between SPME-GC Analysis and the Aroma Intensity for Ginseng Volatiles (SPME-GC를 이용한 인삼의 향분석과 관능강도와의 상관관계)

  • Ryu, Sung-Kwon;Roh, Jin-Chul;Park, Hoon;Park, Sung-Kook
    • Journal of Ginseng Research
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    • v.26 no.4
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    • pp.206-212
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    • 2002
  • Ginsengs grown fur six years at different locations were harvested and prepared for white and red ginsengs. These fresh, white, red, and other ginsengs purchased from domestic and foreign countries were analyzed for their volatile compounds by solid phase microextraction-gas chromatography (SPME-GC) and SPME-GC/mass spectrometery (MS). The intensity of the ginseng volatiles perceived by nose was also measured in order to correlate the intensity with the corresponding GC analysis. Good correlations were obtained between the GC peak area and the degree of intensity evaluated by sensory panelists, indication that a reliable and objective evaluation of the aroma intensity of ginsengs by a simple GC analysis is possible.

Development of Analytical Technology Using the HS-SPME-GC/FID for Monitoring Aromatic Solvents in Urine

  • Lee, Mi-Young;Chung, Yun Kyung;Shin, Kyong-Sok
    • Mass Spectrometry Letters
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    • v.4 no.1
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    • pp.18-20
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    • 2013
  • Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque (고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법)

  • Ahn Sang-Woo;Lee Si-Jin;Chang Soon-Woong
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.

Analysis of the composition of trail pheromone secreted from live Camponotus japonicus by HS-SPME GC/MS (HeadSpace-Solid Phase MicroExtraction Gas Chromatography/Mass Spectrometry) (HS-SPME GC/MS법을 이용한 일본왕개미의 trail pheromone 성분 분석)

  • Park, Kyung-Eun;Lee, Dong-Kyu;Kwon, Sung Won;Lee, Mi-Young
    • Analytical Science and Technology
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    • v.25 no.5
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    • pp.292-299
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    • 2012
  • GC/MS has been utilized for many applications due to great resolution and reproducibility, which made it possible to build up the database of mass spectrum, while HS-SPME has the advantage of solventfree extraction of volatile compounds. The combination of these two methods, HS-SPME GC/MS, enabled many scientific applications with various possibilities. In this study, the analysis of trail pheromone excreted from live Camponotus japonicus with the feature of solvent-free extraction was carried out and the optimization for this analysis was performed. The major compounds detected were n-decane, n-undecane, and n-tridecane. Optimization for the best detection of these hydrocarbons was processed in the point of SPME parameter (selection of fiber, extraction temperature, extraction time, etc.). The advantage of the analysis of live sample is to analyze phenomenon right after it is excreted by ants. But the experimental process has restriction of extraction temperature and time because of the analysis of live ants. Establishing the process of HS-SPME GC/MS applied to live samples shown in this study can be a breakthrough for the ecofriendly and ethical research of live things.

Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS (HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법)

  • Rhee, Jong-Sook;Jung, Jin-Mi;Lee, Han-Sun;Yeom, Hye-Sun;Lee, Sang-Ki;Park, Yoo-Sin;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.54 no.6
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    • pp.429-440
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    • 2010
  • HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Determination of DBCP and n-Butylbenzene using SPME with GC-MS (SPME-GC-MS를 이용한 DBCP 및 n-Butylbenzene의 분석)

  • Park, Hyun-Mee;Kim, Young-Man;Lee, Dai-Woon;Lee, Kang-Bong
    • Analytical Science and Technology
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    • v.14 no.6
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    • pp.471-475
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    • 2001
  • Solid phase microextraction(SPME) with $85{\mu}m$-polyacrylate (PA) and $100{\mu}m$-polydimethylsiloxane(PDMS) fibers, coupled to gas chromatography-mass spectrometry was used to determine 1,2-dibromo-3-chloropropane(DBCP) and n-butylbenzene in water. The conditions affecting the SPME process(i.e, extraction time, injection length, injection temperature, desorption time and temperature) were optimized. The linearity of the calibration curve (correlation coefficient, R) was over 0.99 and the limits of detection of the method were between 1.5 and $10.8{\mu}g/L$. Repeatability of the method was between 10.4 and 14.4 %.

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Flavor Characteristic of Functional Modified-butterfat Synthesized by Lipase-catalyzed Interesterification (효소적 공법을 이용한 기능성 modified-butterfat의 향기성분 특성 분석)

  • Shin, Jung-Ah;Lee, Ki-Teak
    • Korean Journal of Agricultural Science
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    • v.36 no.2
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    • pp.219-224
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    • 2009
  • Two functional modified-butterfats (MF668 and MF866) were synthesized with two blends (6:6:8 and 8:6:6, w/w%) of anhydrous butterfat (ABF), palm stearin (PS) and flaxseed oil (FSO, omega-3) via lipase-catalyzed interesterification reaction. Their flavor characteristic was investigated using electronic nose and SPME-GC/MS analysis. Each flavor pattern of ABF, FSO, MF668 and MF866 was significantly discriminated with first principal component score of 95.16% in PCA plot. In functional modified-butterfats analyzed with SPME-GC/MS, various volatile compounds such as aldehydes, ketones, acids, and alkanes were detected.

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Analysis of Flavor-related Compounds from Tobacco using SPME-GC-MS (SPME-GC-MS를 이용한 담배와 관련된 향료의 분석)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.109-114
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    • 2001
  • The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry(GC-MS). Flavor-related compounds were estragole pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin. More than on of the flavor-related compounds were detected in the range $0.001-1.3{\mu}g/g$ from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%.

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