• Korean Journal of Food Science and Technology
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• v.37 no.3
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• pp.339-344
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• 2005

Volatile compounds, isolated from Elsholtzia splendens using simultaneous steam distillation extraction (SDE) and headspace solid phase microextraction (HS-SPME), were analyzed by gas chromatography/mass spectrometry(GC-MS). Twenty-nine compounds, comprising 3 aldehydes, 7 alcohols, 11 hydrocarbons, 5 ketones, and 3 miscellaneous ones, were tentatively identified from volatile compounds of Elsholtzia splendens flowers. From leaves, 30 compounds, comprising 3 aldehydes, 6 alcohols, 11 hydrocarbons, 6 ketones, and 11 miscellaneous ones, were tentatively identified. Volatile compounds extracted by HS-SPME in E. splendens flowers were 3 alcohols, 18 hydrocarbons, 3 ketones, and 2 miscellaneous ones. In leaves, 31 compounds, comprising 7 alcohols, 15 hydrocarbons, 7 ketones, and 2 miscellaneous ones, were tentatively identified. Major volatile compounds identified by SDE and HS-SPME were naginataketone and elsholtziaketone, which were identified as aroma-active compounds, representing characteristic aroma of E. splendens.

• Analytical Science and Technology
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• v.19 no.1
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• pp.96-102
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• 2006

Trimethylamine (TMA) is one of the difficult odorous compounds for the collection and analysis. Although sulfuric acid absorption and/or sulfuric acid impregnated filter method are commonly recommended for its sampling, these methods also suffer from difficulties involved in sample treatment and operational procedures. Hence, as an ancillary approach to measure TMA, we investigated the combination of bag sampling and SPME analysis for TMA measurements. For the purpose of our study, we investigated the following three subjects: 1) temporal variability of standard storage, 2) bag loss effect of TMS, and 3) TMA loss due to repetitive analysis of an identical bag sample. According to our storage test up to 7 or 20 dyas, TMA loss were found to occur up to 40 to 50% within relatively short period of up to 48 hrs depending on its concentration ranges. When the tests were made for bag loss by transferring TMA standards across different size bags, we were able to find that the extent of bag loss are not significant with 5 to 20% loss rate. Finally, the TMA sorptive loss via its exposure to SPME fiber was generally estimated to run from 2 to 3%.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2003.09a
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• pp.458-461
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• 2003

Solid-phase microextraction (SPME) and gas chromatography/headspace techniques(HS) and flame ionization detection (GC/FID) have been combined for determination of very polar compounds in water, including the widely used gasoline oxygenates and by-products. A relatively simple extraction method using a CAR/PDMS(75${\mu}{\textrm}{m}$) SPME fiber was optimized for the routine analysis of gasoline oxygenates and by-products in groundwater and reagent water. A sodium chloride concentration of 25%(w/w) combined with an extraction time of 20 min provided the greatest sensitivity while maintaining analytical efficiency Replicate analyses in fortified reagent and groundwater spiked with microgram per liter concentrations of gasoline oxygenates and by-products indicate quantitative and reproducible recovery of these and related oxygenate compounds. Method dynamic range was 50$\mu\textrm{g}$ L-1 to 3000$\mu\textrm{g}$ L-1 for gasoline oxygenates and by-products.

• Journal of the Korean Society of Tobacco Science
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• v.35 no.1
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• pp.7-12
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• 2013

A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.

• ETRI Journal
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• v.32 no.3
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• pp.440-446
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• 2010

Array-based gas sensors now offer the potential of a robust analytical approach to odor measurement for medical use. We are developing a fast reliable method for detection of microbial infection by monitoring the headspace from the infected wound. In this paper, we present initial results obtained from wound-state monitoring for burn patients using an electronic nose incorporating an automated solid-phase microextraction (SPME) desorption system to enable the system to be used for clinical validation. SPME preconcentration is used for sampling of the headspace air and the response of the sensor module to variable concentrations of volatiles emitted from SPME fiber is evaluated. Gas chromatography-mass spectrometry studies prove that living bacteria, the typical infectious agents in clinical practice, can be distinguished from each other by means of a limited set of key volatile products. Principal component analysis results give the first indication that infected patients may be distinguished from uninfected patients. Microbial laboratory analysis using clinical samples verifies the performance of the system.

• Food Science and Biotechnology
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• v.18 no.4
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• pp.895-899
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• 2009

A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.

• Food Science and Biotechnology
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• v.14 no.2
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• pp.238-241
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• 2005

Aroma-active compounds were evaluated from salt-fermented anchovy sauce by solid phase microextraction-gas chromatography-olfactometry (SPME-GC-O) based on sample dilution analysis (SDA). SPME extract from carboxen/polydimethylsiloxane (CAR/PDMS) fiber was the most similar to the original odor of salt-fermented anchovy sauce used for this experiment, followed by divinylbenzene/CAR/PDMS (DVB/CAR/PDMS) fiber. Because salt-fermented anchovy sauce contains 23% NaCl, NaCl concentration of diluent was considered when salt-fermented anchovy sauce was serially diluted. Linear relationship between GC response and sample concentration was observed when diluted with 23% NaCl solution, whereas not observed when diluted with deodorized distilled water. Eleven and 16 aroma-active compounds were detected by SPME-GC-O based on SDA using CAR/PDMS and DVB/CAR/PDMS fibers, respectively. Butanoic acid and 3-methyl butanoic acid showed the highest ${\log}_2SD$ factors for CAR/PDMS and DVB/CAR/PDMS fibers. Dimethyl trisulfide, methional, trimethyl amine, 1-penten-3-ol, and acetic acid were also detected as potent aroma-active compounds.

• Korean Journal of Food Science and Technology
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• v.35 no.3
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• pp.359-365
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• 2003

Headspace solid-phase microextraction(HS-SPME) was used to isolate the off-flavor volatile compounds, which are formed during the oxidation of porcine liver and unsaturated fatty acids in porcine liver induced by iron. Three fibers for HS-SPME method development were tested, and the polydimethylsiloxane/divinylbenzene(PDMS/DVB) fiber was selected as providing the best detection of analyzed compounds. In the oxidized arachidonic acid, the major compounds identified were hexanal, 1-octen-3-one(metallic), (Z)-4-heptenal, (E)-2-octenal, 1-octen-3-ol(mushroom), (Z)-2-nonenal (cardboard-like), and (E,E)-2,4-decadienal(fatty, oily). In the oxidized linolenic acid, the major ones were (E,E)-2,4-heptadienal(fishy), (E,E)-3,5-octadien-2-one and (E,Z)-2,6-nonadienal. Moreover, those of th oxidized porcine liver with iron were hexanal, 1-octen-3-one, (Z)-4-heptenal, (E,Z)-2,4-decadienal and (E,E)-2,4-decadienal. These results showed that the fishy and metallic off-flavor in porcine liver were due to the oxidation of unsaturated fatty acids in porcine liver.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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• 2004.04a
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• pp.354-357
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• 2004

The addition of oxygenates to diesel fuel can significantly reduce particulate emissions. Dibutyl maleate (DBM) and tripropylene glycol methyl ether (TGME) have been identified as possible additives based on their physicochemical characteristics and performance in engine test. However, their potential environmental impacts are unknown. therefore, practical considerations in the selection of an oxygenate additives should include cost, availability, compatibility with engines and fuel, and, particularly, its overall environmental impact. This study was investigated to determine optimal condition for the analysis of potential diesel oxygenates using SPME technique with GC-FID. Four fibers were compared and CAR/PDMS fiber was found to be the most sensitive when used direct-sampling. An absorption time of 30min and a desorption time of 5min provided to be the most sensitivity. The effects of experimental parameters such as the addition of salts, agitation, absorption time, compositon on the analysis were investigated. Analytical parameter such as linearity was also evaluated.

• Analytical Science and Technology
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• v.14 no.1
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• pp.44-49
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• 2001

Solid-phase microextraction (SPME) with $85{\mu}m$ polyacrylate fiber, coupled to gas chromatography-mass spectrometry was used to analyze the plasticizers contained in balloon samples. The balloons were identified to be made of polyisoprene by IR spectroscopy. The plasticizers extracted from the balloon samples soaked in acetone-added water solvent for an hour were quantified by external standard method using nine kinds of plasticizers. The quantification method was validated for standard plasticizers in the range of $0.25-25{\mu}g/g$. The detection limits were $0.11-0.38{\mu}g/g$ for different plasticizers. The RSDs for the reproducibility of this quantitation method were 3.7-14.2%. A few of balloons included risky level of plasticizer concerned as and endocrine disrupter, and it is necessary to regulate these products.