• 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.

• 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.

• Journal of Environmental Science International
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• v.23 no.10
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• pp.1693-1701
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• 2014

A rapid and simple method for the quantitative determination of volatile fatty acids (VFAs; propionic acid, n-butyric acid, i-valeric acid and n-valeric acid) and indoles (phenol, p-cresol, 4-ethyl phenol, indole and skatole) in pig slurry and dog excrement using solid-phase micro-extraction (SPME) coupled to gas chromatography was evaluated. $50/30{\mu}m$ DVB/CAR/PDMS (Divinylbenzene/Carboxen/Polydimethylsiloxane) fiber was used to extract the target compounds in aqueous media. Sample amount and adsorption time was standardized for the routine analysis. Detection limits were from 0.11 to $0.15{\mu}gL$ for VFAs and from 0.12 to $0.28{\mu}gL$ for indoles and the correlations observed ($R^2$) were 0.975~1.000. This method was applied to the pig slurry, fertilizer, compost and dog excrement. In nearly all cases, the indoles were detected in concentrations of higher than their limits of detection (DOLs). But the VFAs in swine manure were below their DOLs.

• Journal of Korean Society for Atmospheric Environment
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• v.23 no.1
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• pp.39-49
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• 2007

In this study, the performance characteristics of solid phase microextraction (SPME) were investigated for three major odorous groups that consist of 10 individual compounds ([1] volatile organic compounds (VOC): benzene, toluene, p-xylene and styrene, [2] reduced sulfur compounds (RSC): hydrogen sulfide, methyl mercaptan, dimethylsulfide (DMS), dimethyldisulfide (DMDS), and carbon disulfide, and [3] amine: trimethylamine (TMA)). For the purpose of a comparative analysis, two types of SPME fiber ([1] polidimethylsiloxane/divinilbenzene (P/D) and [2] $Carboxen^{TM}$/polidimethylsiloxane (C/P)) were test ε d against each other for a series of standards prepared at different concentration levels (100, 200, and 500 ppb). To compare the analytical performance of each fiber, all standards were analyzed for the acquisition of calibration data sets for each compound. The results of P/D fiber generally showed that its calibration slope increased as a function of molecular weight across different VOCs; however, those of C/P fiber showed a fairly reversed trend. Besides, we confirmed that the application of SPME is limited to many sulfur compounds; only two compounds (DMS and DMDS) are sensitive enough to draw calibration results out of SPME. The calibration data for RSC show generally enhanced slop values for C/P relative to P/D fiber. However, in the case of TMA, we were not able to find a notable difference in their performance.

• The Korean Journal of Food And Nutrition
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• v.16 no.4
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• pp.372-378
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• 2003

The volatile components of cinnamon bark were extracted by using different isolation methods, simultaneous distillation extraction (SDE) and solid phase microextraction (SPME). Then the volatile components were analyzed by gas chromatography(GC) and mass selective detector(MSD). 30 compounds were identified in cinnamon bark. In SPME technique, several factors influencing the equilibrium of the aroma compounds between sample and SPME fiber was taken into account, including the kind of SPME fiber, extraction temperature and extraction time. Four different SPME fibers were tested, namely polydimethylsiloxane (PDMS), poly acrylate(PA), divinyl- benzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS) and carbowax/divinylbenzene(CW/DVB). Among these SPME fiber, PDMS coating fiber showed the best results. The profile of volatile compounds of cinnamon bark at different extraction temperature and extraction time were investigated by 100$\mu\textrm{m}$ PDMS fiber.

• Journal of the Korean Society of Tobacco Science
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• v.28 no.2
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• pp.136-143
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• 2006

This study was conducted to determine the amount of unprotonated nicotine in cigarette mainstream smoke and to investigate its relationship to level of filter ventilation and machine smoking conditions. Unprotonated nicotine from TPM trapped on a Cambridge filter pad(CFP) was adsorbed by Carboxen/PDMS SPME fiber, thermally desorbed and determined by GC/MS. 2R4F reference cigarette, twelve commercial brands from the Korean market and five test cigarette samples, which had the same tobacco blend with different levels of filter ventilation, were analyzed for unprotonated nicotine. In commercial brands, the amount of unprotonated nicotine changed slightly depending on the pH values of smoke, and decreased as the tar level increased. filter ventilation in these commercial cigarettes was $28{\sim}80%$ and the higher filter ventilation increased relative unprotonated nicotine levels, but not significantly. However, in five test cigarettes with different filter ventilation$(0{\sim}70%)$, unprotonated nicotine levels increased almost linearly with the level of filter ventilation. Concentrations of unprotonated nicotine in mainstream smoke generally increased in order $HC\;<\;ISO\;{\leq}\;MDPH$ machine smoking conditions. The ratio of unprotonated nicotine to total nicotine among $cigarettes({\alpha}_{fb})$ increased in order RC < MDPB < ISO conditions. Concentrations of unprotonated nicotine varied with three machine smoking conditions.

• Analytical Science and Technology
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• v.17 no.6
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• pp.496-513
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• 2004

This study was carried out to evaluate the performance of sampling and analytical methodology used for the measurement of toxic volatile organic compounds (VOCs) in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/MSD analysis. Target analytes were 33 compounds including major aromatic compounds such as BTEX, and halogenated compounds. The methodology was investigated with a wide range of different adsorbents which are commercially available and have been frequently adopted for the VOC measurement. A total of 10 adsorbents were tested in this study: 6 carbon-based adsorbents such as Carbotrap, Carbopack B, Carbosieve S-III, Carboxen 1000, Carbotrap C, Activated Charcoal; and 4 polymer-based adsorbents including Tenax, Porapak Q, Chromosorb 102, and Chromosorb 106. The sampling performance was evaluated with respect to the sampling capacity of VOCs with single-adsorbent and multiple-adsorbents methods for standard samples and field samples. As a result, the best adsorbents for single-adsorbent method in the sampling of toxic organic compounds (including benzene, toluene, xylenes etc.) appeared to be Carbotrap, Carbopack B and Tenax TA. On the other hand, Chromosorb 102, Chromosorb 106 and Porapak Q were found to be unsuitable adsorbents for VOC measurement based on thermal desorption method. Multi-adsorbent packings were evaluated with 4 carbon-based adsorbents, which classified by 3 combination sets of double adsorbents and 2 combination sets of triple adsorbents. The results indicated that the most suitable combination for toixc VOC measurements is Carbotrap C with Carbotrap. Multi-sorbents tubes packed with a strong adsorbent such as Carbosieve S-III or Carboxen 1000 were found to be relatively unsuitable for several compounds, not only owing to the effect of migration of adsorbed compounds from weaker adsorbent to stronger adsorbent, but to hydrophobic nature of the adsorbents. Therefore, it should be addressed that selection of a proper adsorbent (or combination of multi sorbents) is extremely important to obtain reliable data for the concentrations of toxic VOCs in indoor and outdoor environments.

• Journal of Korean Society for Atmospheric Environment
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• v.23 no.5
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• pp.547-556
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• 2007

The release, sampling and analytical methods have been developed and tested for perfluorocarbons (PFCs) atmospheric tracers in order to gain insight into the atmospheric transport and dispersion over the urban conditions of Seoul, Korea. Although PFCs tracer experiments provide unique opportunities to test local and urban scale of transport and dispersion, no previous experiment with PFCs has been conducted in Korea. PMCH and PDCH were chosen as targeted tracers in our study due to their extreme low ambient concentrations and great sensitivities among various PFCs. For PFCs release system, a set of micro-metering pump, electronic balance, vaporizing furnace and high speed blower was constructed for precise and accurate release of tracers. The precision of released rate by this system was estimated to be 1%. Samplings of PFCs were carried out by fabricated portable air samplers with micro pumps and rotameters into glass tubes packed with 150 mg of Carboxen-569. The uncertainty of these sampling system was maintained below 14%. PMCH and PDCH were quantified in GC/ECD with preconditioned injection system to eliminate the interference compounds using traps and subsequent catalytic conversion system prior to column separation. Three intensive field test were undertaken during the springtime of 2002 to 2004 in eastern part of Seoul. Daily background samples were collected to characterize the background levels of PMCH and PDCH prior to their release. The observed background concentrations of PMCH ranged from 3.5 to 10.1 fL/L and varied randomly in location and time in this study. Its mean and standard variation of background concentration ($6.8{\pm}1.9\;fL/L$) are higher than those ($3.2{\sim}5.8\;fL/L$) of other historic tracer studies. Identified uncertainty for background PMCH was $1.7{\sim}2.0\;fL/L$ using this analytical system. Combined relative uncertainty in determining the tracer's concentrations was estimated as 17%. However, its background concentrations and uncertainty in concentration determination were found to be low and stable enough for tracer study.

• 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.

• Analytical Science and Technology
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• v.21 no.2
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• pp.93-101
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• 2008

The application of solid phase microextraction (SPME) is generally conducted by directly immersing the fiber into the liquid sample or by exposing the fiber in the head space (HS). The extraction temperature, the time of incubation, and application of stirring are often designated to be the most important parameters for achieving the best extraction efficiencies of HS-SPME analysis. In this study, relative importance of these three analytical parameters involved in the HS-SPME method is evaluated using a polydimethylsiloxane/carboxen (PDMS/CAR) fiber. To optimize its operation conditions the competing relationships between different parameters were investigated by comparing the extraction efficiency based on the combination of three parameters and two contracting conditions: (1) heating the sample at 30 vs. 50 C, (2) exposing samples at two durations of 10 vs. 30 min, and (3) application of stirring vs. no stirring. According to our analysis among 8 combination types of HS-SPME method, an extraction condition termed as S50-30 condition ((1) 1200 rpm stirring, (2) $50^{\circ}C$ exposure temp, and (3) 30 min exposure duration) showed maximum recovery rate of 45.5~68.5% relative to an arbitrary reference of direct GC injection. According to this study, the employment of stirring is the most crucial factor to improve extraction efficiency in the application of HS-SPME.