• Journal of Soil and Groundwater Environment
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• v.15 no.1
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• pp.9-18
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• 2010

In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

• Analytical Science and Technology
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• v.20 no.5
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• pp.370-382
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• 2007

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

• Food Science of Animal Resources
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• v.33 no.5
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• pp.646-654
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• 2013

In this study, quantitative analysis of major volatile flavor compounds from yogurt was conducted using headspace-solid phase microextraction (HS-SPME) GC-FID analysis technique, and the changes of volatile aroma compounds during the storage period were evaluated. The yogurt was prepared with the addition of 2% cereals, such as, white rice (WR), brown rice (BR), germinated brown rice (GBR) and saccharified germinated brown rice (SGBR). After fermentation, the products were stored at $5^{\circ}C$for 15 d. The major volatile aroma compounds in yogurt, such as acetaldehyde, acetone, diacetyl and acetoin were able to be extracted using HS-SPME technique efficiently. The regression ($r^2$) value of standard curve prepared with various concentrations of individual flavor chemicals was analyzed over 0.9975, and reproducibility was acceptable to apply quantitative analysis. The analysis of volatile components of control sample during storage showed that the acetaldehyde on 0 d was 10.83 ppm, and that contents were increased to 15.67 ppm after 15 d of storage. However, addition of BR, GBR and SGBR decreased the acetaldehyde contents during storage periods. The acetone content of all treatments during storage was not significantly different. The diacetyl content of all treatments were increased during storage and the addition of SGBR showed the highest amount of diacetyl (0.84 ppm) among treatments on 15 d of storage. The acetoin content of yogurt added with grains was higher than that of control during storage. As a result, the content of volatile aroma compounds in yoghurt during storage period could be analyzed HS-SPME extraction technique effectively, and HS-SPME/GC analysis can be considered for quality control of fermented milk products.

• 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.

• Journal of the Korean Chemical Society
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• v.48 no.1
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• pp.17-27
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• 2004

A procedure based on solid phase microextraction extraction(SPME)-GC/MS has been developed for the simultaneous analysis of plasticizers. The plasticizers investigated in this study are dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP), benzylbutyl phthalate(BBP), diethylhexyl phthalate (DEHP), di-n-octyl phthalate(DnOP). The limit of detection(LOD) was 0.163~0.299 with relative standard deciation(RSD) of 5.85~15.80% for these compounds. At water reserviors of Han, Geum, Nakdong and Sumjin rivers, only DBPand DEHP were detected at trace level, 0.192~1.270 ng/ml for DBP and 0.077~1.102 ng/ml for DEHP depending on the river.

• 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.

• Journal of Korean Society for Atmospheric Environment
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• v.24 no.3
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• pp.357-366
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• 2008

In this study, the analytical performance of trimethylamine (TMA) were investigated with respect to headspace-solid phase microextraction (HS-SPME) method. In order to induce the elution of aqueous TMA to headspace, NaOH was added as a decomposition reagent to aqueous TMA standard. By controlling the combination of three major variables for TMA extraction, the extent of extraction was compared between the two contrasting conditions for each variable (i.e., reaction time (long (L) vs short (S)), exposure temperature (30 vs $50^{\circ}C$), and exposure time (10 vs 30 min)). The results of this comparative analysis showed that the extraction efficiency for all eight types of HS-SPME combinations decreased on the order: L-30-30>L-50-10>L-30-10>L-50-30>S-30-30>S-50-30>S-50-10>S-30-10. The effect of reaction time appeared to exert significant influences on the relative recovery rate of HS-SPME at 90% confidence level. However, the effects of exposure temperature or exposure time were not so significant as reaction time. When the recovery rate of HS-SPME is compared against the direct injection of liquid standard into GC injector, it recorded as 2%. According to this comparative study, the reaction conditions for HS-SPME application can exert significant influences on the analysis of TMA.

• Korean Journal of Food Science and Technology
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• v.32 no.3
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• pp.507-512
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• 2000

The headspace flavors of roasted tea, prepared with steamed and nonsteamed polygonatum roots, were absorbed in solid-phase microextraction(SPME) fiber coated with $65\;{\mu}m$ of carbowax/divinylbenzene(CW/DVB) and analysed by GC-MS. The absorption conditions of SPME fiber for equilibrated headspace were selected as $60^{\circ}C$ and 30 min. In a comparison for both samples roasted at $130^{\circ}C$ for 15 min, gas chromatograms showed a similar pattern in overall profiles between steamed and nonsteamed samples before roasting, but some differences were observed in peak characteristics. From 40 separated peaks, 25 compounds were identified with both GC-MS and retention time comparison. The pyrazines including 2,3-dihydro-3,5-dihydroxy-6-methyl-4H-pyran-4-one, 2,5-dimethyl-4-hydroxy-3(2H)-furanone, 2-acetyl-1-pyrroline, etc. were higher in their contents in nonsteamed-roasted sample than steamed-roasted one. In particular, steamed-roasted polygonatum showed higher contents of acetic acid(8.17%) and hexanoic acid(5.43%) than the corresponding compounds of nonsteamed-roasted one, 2.40% and 2.00%.

• Journal of Environmental Science International
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• v.22 no.12
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• pp.1539-1549
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• 2013

The purpose of this study is to compare the sampling methods for monitoring indoles (phenol, p-cresol, indole and skatole) in airs of swine facility. As the collecting methods of indoles in air, Tenax-TA adsorption tube and solid phase microextraction (SPME) were examined. For the preparation of calibration curves of indoles concentrated in Tenax-TA, the standard indoles solutions were spiked in each of Tenax-TA tubes and thermally desorbed (ATD) into a gas chromatograph combined with mass detector (GC/MS). And for the preparation of calibration curves by SPME, indoles in the standard gaseous solution prepared by evaporating the aqueous solution that contained indoles into a polyester sampling bag were extracted with SPME fiber and subsequently analyzed by the GC/MS. Two sampling methods were evaluated for extracting indoles present in swine building environments. Results indicated that the SPME method using Polydimethylsiloxane/ Divinylbenzene (PDMS/DVB) fiber was more effective than Tenax-TA method in extracting indoles. The gas chromatographic analysis showed that the linearities of calibration curves and detection limits were useful for detection of indoles in swine airs. The field tests also showed that considerably different levels of indoles were present in various parts of the swine building.