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Partitioning Behavior of Selected Printing Ink Solvents between Headspace and Chocolate Cookie Samples

  • An, Duek-Jun
    • Preventive Nutrition and Food Science
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    • v.16 no.3
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    • pp.267-271
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    • 2011
  • Static Headspace Gas Chromatographic analysis was used to study the partitioning behavior of five organic printing ink solvents between chocolate cookie/air systems. Three cookie sample formulations varied with respect to chocolate type and overall percentage of constituents. Major considerations involved differences in fat content and type and resulting variability in chemical and physical structure. Each of the solvents studied (ethyl acetate, hexane, isopropanol, methyl ethyl ketone, toluene) represents a general class of printing ink solvents based on predominate functional group. Values of the partitioning coefficient (Kp) were determined at equilibrium using measured quantities of both solvent and cookie sample in closed systems at temperature of 25, 35, and $45^{\circ}C$. In each of the three cookies at the three test temperatures, toluene always exhibited the greatest value of partitioning to cookie and hexane always exhibited the least. Results also showed that the partitioning behavior of solvents is generally inversely related to temperature and that solvent affinity, though constant for a particular cookie type over all test temperatures, varies significantly among the three cookie types. The preference of each of the five solvents for each cookie sample was also found to vary with temperature. No correlation was found between the extent of partitioning and cookie formulation or physical characteristic of solvent. The Hildebrand parameter, related to ${\Delta}Hmix$ (heat of mixing), may be used to describe differences in partitioning based on the overall potential of a solvent/cookie interaction to occur. The potential for interaction is dependent upon the chemical structure of the cookie sample and thus the availability of 'active-sites' required for a given solvent.

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 Volatile Organic Compounds in Waste using HS/GC/MS Analysis (Headspace/GC/MS를 이용한 폐기물중 휘발성 유기화합물의 분석)

  • Kim, Kyeo-Keun;Shin, Sun-Kyoung;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.72-80
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    • 2000
  • The HS/GC/MS method was performed to analyze the volatile organic compounds in waste sludge samples. This study was performed to establish the fundamental data by studying the effects of salt, equilibrium temperature and time in the volatile organic compounds analysis. The presence of salts have been found to increase the sensitivity. The peak area is increased from 1.07 to 2.61 times by adding the salts to the water sample, compared with a salt tree sample. The recoveries of target compounds have found between 90% and 127% at sample temperature of $85^{\circ}C$ for 30 min. This HS/GC/MS method can be applied to analyze the volatile organic compounds and organohalo compounds in the environmental matrix.

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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.

Effects of Malotilate on Levels of Ethanol and Acetaldehyde in Blood (혈중 Ethanol 및 Acetaldehyde의 농도에 미치는 Malotilate의 영향)

  • 허인회;이상준;주왕기;허문영;김형춘;송계용
    • YAKHAK HOEJI
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    • v.31 no.6
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    • pp.399-401
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    • 1987
  • A gas chromatographic utilizing procedure headspace gas analysis is performed to study effect of malotilate on levels of ethanol and its metabolite acetaldehyde in a blood sample from the rat. The concentrations of ethanol and acetaldehyde were determined simultaneously at 1, 3, and 6h after ethanol administration. Our results would suggest the malotilate could promote clearances of ethanol and acetaldehyde in blood, and could accelerate it, especially, in $CCl_4$ pretreated rats.

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Competitive Extraction and Trace Analysis of BTEX and MTBE by Solid-Phase Microextraction (SPME) (고체상미량추출법을 이용한 BTEX와 MTBE의 경쟁적 추출효과 및 미량분석에 관한 연구)

  • An, Sang-Woo;Chun, Suk-Young;Lee, Si-Jin;Park, Jae-Woo;Chang, Soon-Woong
    • Journal of Korean Society on Water Environment
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    • v.26 no.4
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    • pp.622-628
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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 BTEX and MTBE. 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 50 mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of BTEX and MTBE. The general affinity of analytes to CAR/PDMS fiber was high in the order p-Xylene>Toluene>Ethylbenzene>MTBE>Benzene. The linearity of $R^2$ for BTEX and MTBE was from 0.970 to 0.999 when analyte concentration ranges from $30{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.5% to 3.2% for concentration of $100{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for BTEX and MTBE were from $7.5{\mu}g/L$ to $15{\mu}g/L$, respectively.

Analysis of tert-Butanol, Methyl tert-Butyl Ether, Benzene, Toluene, Ethylbenzene and Xylene in Ground Water by Headspace Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Kim, Tae-Seung
    • Bulletin of the Korean Chemical Society
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    • v.30 no.12
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    • pp.3049-3052
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    • 2009
  • Methyl tert-butyl ether (MTBE) is added to gasoline to enhance the octane number of gasoline, tert-butyl alcohol (TBA) is major degradation intermediate of MTBE in environment, and benzene, toluene, ethyl benzene and xylene (BTEX) are also major constituents of gasoline. In this study, a simplified headspace analysis method was adapted for simultaneous determination of MTBE, TBA and BTEX in ground water samples. The sample 5.0 mL and 2 g NaCl were placed in a 10 mL vial and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was placed in a heating block at 85 $^{\circ}C$ for 30 min. The detection limits of the assay were 0.01 ${\mu}$g/L for MTBE and BTEX, and 0.02 ${\mu}$g/L for TBA. The method was used to analyze 110 ground water samples from various regions in Korea, and to survey the their background concentration in ground water in Korea. The samples revealed MTBE concentrations in the range of 0.01 - 0.45 ${\mu}$g/L (detection frequency of 57.3%), TBA concentrations in the range of 0.02 - 0.08 ${\mu}$g/L (detection frequency of 5.5%), and total BTEX concentrations in the range of 0.01 - 2.09 ${\mu}$g/L (detection frequency of 87.3%). The developed method may be used when simultaneously determining the amount of MTBE, TBA and BTEX in water.

Quantification of Volatile Organic Compounds in Gas Sample Using Headspace Solid-Phase Microextraction (고상 미세 추출법을 이용한 가스시료 중 휘발성유기화합물의 정량 분석)

  • Kim, Jae Hyuck;Kim, Hyunook
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.12
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    • pp.906-917
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    • 2013
  • The purpose of this study is to quantify volatile organic compounds (VOCs) in gas sample using headspace solid-phase microextraction (HS-SPME) coupled to GC analysis. The optimal HS-SPME conditions was CAR/PDMS fiber and 30 min absorprion time for the analysis of various VOCs. In optimal conditions, 80 VOCs could be detected within 1 ppbv and even less than 0.0005 ppbv especially in the case of BTEX. However, fiber reproducibility on adsorption efficiency was 1~9.2% (between the same fiber) and 5.9~13.5% (between the other fiber). We successfully determined 35 VOCs in landfill gas with this method and found that VOCs of high concentration are emitting from vent pipe of closed/open landfill site under the HS-SPME conditions. This method may apply to VOCs/odor determination from various atmospheric environmental samples as well as landfills.

Effects of Heating Time and Storage Temperature on the Oxidative Stability of Heated Palm Oil (가열시간과 저장온도가 가열팜유의 산화안정성에 미치는 영향)

  • Choe, Eun-Ok
    • Korean Journal of Food Science and Technology
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    • v.29 no.3
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    • pp.407-411
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    • 1997
  • Effects of heating time and storage temperature on the oxidative stability of heated palm oil were studied. Palm oil was heated at $150^{\circ}C$ for 0, 1, 10 or 20 min and stored at 4, 20 or $65^{\circ}C$. The oxidative stability of the sample was evaluated by determining peroxide value of the oil and measuring the volatiles in the headspace of the sample. Significant difference in the peroxide or volatile formation was observed (p<0.05) in heated palm oils between samples stored at 4 or $20^{\circ}C$ and those stored at $65^{\circ}C$. Pentane, hexanal, heptane and total volatiles increased with heating time, while storage temperature did not significantly affect their formation, indicating that heating time played more important role in volatile formation in the heated palm oil than storage temperature. However, adverse results were observed for the formation of peroxide. The interaction effect of heating time and storage temperature on the oxidative stability of heated palm oil was also observed.

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Mulberry Paper Bag μ-Solid Phase Extraction for the Analysis of Five Spice Flavors by Gas Chromatography-Mass Spectrometry

  • Yoon, Ok-Kyung;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.35-42
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    • 2009
  • Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.