• Title/Summary/Keyword: Headspace

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Study of the Presence of Residual Hexane in Olive Oils (유통 올리브유의 잔류 헥산에 대한 연구)

  • Kim, Nam-Sook;Lee, Jeung-Hee;Heo, Ok-Soon;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.35 no.10
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    • pp.1405-1411
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    • 2006
  • The presence and content of residual hexane in the olive oils were studied. Total 41 olive oils of imported and domestic brands, which were labeled as extra virgin and refined (mixed), were collected from the market. For analysis, electronic nose and headspace SPME-GC/MS were used. Electronic nose equipped with 12 metal oxide sensors was used for the discrimination of odor pattern of olive oils against the different concentrations of hexane. From the results, it is assumed that the contents of residual hexane in the collected olive oils were below 5 ppm. For Qualitative and quantitative analysis of hexane, polydimethylsiloxane (PDMS) fiber was employed for SPME-GC/MS. In the results, the peak of residual hexane was detected in 8 samples from 41 olive oils. But the detected level was no more than 1 ppm that is under the regulation limit (5 ppm) by Korea Food Additive Code.

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.

Evaluation of TVOC contribution from Raw materials of PVC wallpaper using the Headspace-SPME-GC/MS (HS-SPME-GC/MS 법을 이용한 PVC벽지 원자재의 TVOC 기여도 평가)

  • Jang, Mi-Ok;Jeong, Tak-Kyo;Jeong, Yung-Rim;Kim, Man-Goo
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.488-495
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    • 2007
  • A wallpaper having many surfaces in indoor is composed of various raw materials. In this study, TVOC contribution from raw materials of PVC wallpaper was evaluated by using headspace-solid phase microextraction (HS-SPME)-GC/MS. Samples were diluent, resin stabilizer, plasticizer, filler, blowing agent and PVC resin. 9 mL of each sample was put into 22 mL glass vial and they were equilibrated for 1 hour at $100^{\circ}C$. Headspace in vial was absorbed to $75{\mu}m$ Carboxen-PDMS fiber and analyzed by GC/MS. Aromatic compounds like a toluene, ethylbenzene and xylene, ketones compounds like a acetone, methoxyacetone and 2-butanone and alkane compounds like a nonane decane and undecane were identified from raw materials. And alcohol compounds like a ethanol and butanol and aldehydes were detected. TVOC emission of diluent, resin stabilizer, plasticizer, PVC resin, blowing agent and filler were $54.20{\mu}g/g$, $32.88{\mu}g/g$, $0.50{\mu}g/g$, $0.88{\mu}g/g$, $0.22{\mu}g/g$ and $0.11{\mu}g/g$, respectively. Contribution of TVOC emission of diluent, resin stabilizer and PVC resin that were concerned about add ratio were 0.708, 0.129, 0.115, respectively. In conclusion, it's necessary to reduce TVOC emission through improvement of diluent, resin stabilizer and PVC resin. Also, HS-SPME-GC/MS method which was developed in this study will be used for raw materials analysis effectively.

Henry′s constants of TCE and PCE in surfactant solutions

  • 양중석;백기태;권태순;양지원
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2004.04a
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    • pp.315-317
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    • 2004
  • Henry's law constants of trichloroethylene (TCE) and tetrachloroethylene (PCE) in air-aqueous surfactant systems were determined by gas chromatography headspace analysis of closed system. The effect of surfactant type and concentration was investigated.

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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.

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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Comparative Analyses of the Flavors from Hallabong (Citrus sphaerocarpa) with Lemon, Orange and Grapefruit by SPTE and HS-SPME Combined with GC-MS

  • Yoo, Zoo-Won;Kim, Nam-Sun;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.271-279
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    • 2004
  • The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.