• Journal of Korean Society of Water and Wastewater
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• v.18 no.5
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• pp.638-648
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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 haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

• Food Science of Animal Resources
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• v.30 no.1
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• pp.73-86
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• 2010

The current study was designed to optimize solid phase microextraction (SPME)-GC-MS conditions for extraction and analysis of volatile components for Hanwoo beef and to establish a tentative database of flavor components. Samples were taken from Hanwoo longissimus muscle (30 mon old steer, $1^+B$ carcass grade) at 24 h postmortem. Results indicated that the optimum adsorption time for $75{\mu}m$ CAR/PDMS fiber was 60 min at $60^{\circ}C$. Thermal cleaning at $250^{\circ}C$ for 60 min was the best practice for decontamination of the fiber. A short analysis program with a sharp oven temperature ramp resulted in a better resolution and higher number of measurable volatile components. With these conditions, 96 volatile compounds were identified with little variation including 22 aldehydes, 8 ketones, 31 hydrocarbons, 12 alcohols, 8 nitrogen- and sulfurcontaining compounds, 5 pyrazines and 10 furans. A noticeable observation was the high number of hydrocarbons, aldehydes, ketones, alcohols and 2-alkylfurans which were generated from lipid decomposition especially the oxidation and degradation of unsaturated and saturate fatty acids. This implies that these compounds can be candidates for flavor specification of highly marbled beef such as Hanwoo flavor.

• Journal of the Korean Society of Tobacco Science
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• v.30 no.2
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• pp.117-124
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• 2008

A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

• 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.

• 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.

• Journal of Soil and Groundwater Environment
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• v.12 no.5
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• pp.73-85
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• 2007

In this study, the experiment of solid-phase microextraction (SPME) technique using GC/FID was conducted as a possible alternative to liquid-liquid extraction for the analysis of EGBE, DGBE, DBM and TGME in water, and also, an optimization condition of trace analysis for disel oxygenates including EGBE by the design of experiment (DOE) was described. Experiments used a fractional factorial design method followed by central composite design allowing optimization of a number of factors as well as statistical analysis of the results. The response surface analysis showed that the extraction efficiency could be represented by a second-order polynomial equation in which the salts concentration, extraction temperature, extraction time and sonication time are the major influences. Using DOE method, a new datadependent method was developed to improve the quantity of confidently analyzed disel oxygenates in water samples.

• 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.

• Analytical Science and Technology
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• v.26 no.5
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• pp.299-306
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• 2013

Pyroligneous liquor as a byproduct from charcoal production of bamboo sprout produced damyang-gun has the broad benefits such as improvement of soil quality, plant growth control and is mainly used for the treatment of atopic dermatitis, fungi and many other skin diseases. In this study, flavor compounds of pyroligneous liquor from bamboo sprout produced in Damyang-gun were analyzed and compared using three different methods including direct analysis (DA), headspace solid phase microextraction (HS-SPME) and stir bar sorptive extraction (SBSE). Simultaneously, the analytical conditions of GC-MS for the determination of volatile compounds were optimized. Based on volatile organic compounds detected by GC-MS, SBSE and SPME methods showed higher sensitivity than direct analysis. Major compounds of pyroligneous liquor were cresol, guaiacol, p-ethyl guaiacol and syringol. These phenolic compounds are reported as the useful chemicals with medicinal activity.

• Korean Journal of Food Science and Technology
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• v.43 no.4
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• pp.407-412
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• 2011

Free and bound aroma compounds in green and fermented teas treated with microbial-fermentation were analyzed using headspace-solid phase microextraction gas chromatography (GC) and GC-mass spectrometry. Aldehydes and ketones in green tea decreased during microbial fermentation, whereas linalool and geraniol increased in the fermented tea. After enzyme treatment, (Z)-3-hexen-1-ol increased significantly following enzymatic hydrolysis of both green and fermented teas. In addition, benzaldehyde, 3-hexenyl acetate, and geraniol also increased in green tea with enzyme treatment. Bound aroma compounds in the green and fermented teas increased at different levels of added enzyme. We demonstrated the enhancement of both green and fermented teas by enzyme treatment, which can lead to improvement in the flavor qualities of green and fermented teas.

• Journal of Life Science
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• v.16 no.7 s.80
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• pp.1243-1249
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• 2006

Volatile flavor compounds in commercial crab-like flavorants were compared by mean of solid phase microextraction(SPME) and liquid continuous extraction (LLCE)/GC/MSD methods. A total of 86 volatile flavor compounds were detected. Of these, 71 were positively identified consisting mainly of sulfur-containing compounds (13), aldehydes (3), ketones (2), esters (26), alcohols (5), aromatic compounds (3), terpenes (8), acids (2) and miscellaneous compounds (9). SPME method was more effective than LLCE method in detection of volatile components in commercial crab-like flavorants. Eight S-, N-containing compounds such as dimethyl sulfide, dimethyl disulfide, dipropyl disulfide, 3-(methylthio)propyl acetate, 3-(methylthio) propanal, 3-(methylthio) propanol, 2-methyl-3-(methylthio) pyrazine and 2-methyl-5-(methylthio) pyrazine, 8 esters such as styrallyl acetate, ethyl acetate, isoamyl acetate, benzyl acetate, ethyl pentanoate, butyl pentanoate, isoamyl pentanoate and furfuryl acetate were considered as major components in crab-like flavorants.