• Analytical Science and Technology
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• v.25 no.1
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• pp.39-49
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• 2012

A method to detect 37 volatile organic compounds (VOCs) in surface water was described based on headspace solid-phase micro extraction and gas chromatography-mass spectrometry. VOCs in water were vaporized for 30 min at 40 $^{\circ}C$ in a headspace vial and adsorbed on 85 ${\mu}m$ carboxen-polydimethylsiloxane. Under the established condition, the lowest quantification limit was 4.1-96 ng/L by using 4.0 mL water sample, and the relative standard deviation was less than 15% at concentrations of 0.05 and 0.50 ${\mu}g/L$. The detection limits meet lower concentration than 1/10 of the water quality criteria for VOCs established by the US EPA or Germany. The LOQ is a sensitivity which the monitoring for the establishing water quality criteria requires. When the proposed method was used to analyze the target compounds in sixteen surface water samples and total 16 VOCs were detected in surface water samples collected from Gum-River. Maximum concentrations of VOCs detected were not exceeded the EPA or Germany guidelines in any of the samples.

• 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.

• Applied Biological Chemistry
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• v.31 no.3
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• pp.292-297
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• 1988

The volatiles of whole and homogenated tomato fruits collected by the headspace trapping method using Tenax GC and the simultaneous steam distillation method were identified by GC and GC-MS. Among over 100 GC peaks, 10 alcohols, 6 aldehydes, 4 ketones, 3 esters, 1 phenol and 1 acid were identified from whole tomato fruits, whereas 12 alcohols, 6 aldehydes, 5 ketones, 5 esters, 2 phenols, 1 hydrocarbon and 1 acid were identified from homogenated tomato fruits. By simultaneous steam distillation-extraction, 19 alcohols, 13 hydrocarbons, 9 esters, 9 ketones, 8 aldehydes, 2 phenols, 2 lactones,2 furans, 1 acids and 2 others were identified among over 300 peaks.

• Bulletin of the Korean Chemical Society
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• v.32 no.10
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• pp.3603-3609
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• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• Proceedings of the Korean Society of Food Hygiene and Safety Conference
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• 2001.10a
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• pp.140-140
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• 2001

A sensitive analytical method based on gas chromatograpy-mass spectrometry with a selected ion monitoring (GC/MS-SIM) with the purge-and-trap concentration and with headspace method (in limited applications) was developed for determining of epichlorohydrin in canned beverages coated with epoxy resin. The calibration curve in the range of $0.5\sim50ng$ had correlation coefficient greater than 0.998 and a detection limit of $0.l\mug/L$ was obtained using a sample volume of 20ml. The predominant ions of epichlorohydrin produced in MSD using electron ionization(EI) were m/z 57 ([M-CI]+) and 62/64 $([M-CH_2O]+)$. In survey of epichlorohydrin in thirty commercial canned beverage samples, none of them was detected.

• Journal of the Korean Chemical Society
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• v.25 no.1
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• pp.30-37
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• 1981

A simple micro-sampling system is described which facilitates isolation and concentration of complex organic constituents into three fractions of different volatilities. The method involves the headspace trapping of very volatile components from a complex matrix onto a porous polymer, Tenax GC, followed by the solvent elution of the matrix and the subsequent fractions of the eluate into volatile and less-volatile fractions. The headspace and the volatile fractions are then analyzed by high-resolution capillary gas chromatography. The less-volatile fraction is analyzed by high-performance liquid chromatography. Experimental details and the results obtained using tobacco leaves as a complex organic matrix are presented.

• Korean Journal of Food Science and Technology
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• v.28 no.1
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• pp.15-18
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• 1996

Twenty different kinds of roasted and ground coffees, 9 domestic and 11 foreign coffee products, were analyzed using a headspace gas chromatographic technique. Among many aroma compounds, acetaldehyde, acetone, carbon disulfide, isobutylaldehyde, 2-methylfuran, 2-methylbutanol and isovaleraldehyde were mainly analyzed for aroma pattern. Roasting color was determined by Photovolt colorimeter. The average roasting color of the foreign coffee was 54 and 47 for domestic coffee. It means that color of the domestic coffee was darker than that of the foreign coffee. The correlation of coefficient between roasting color and 2-methylfuran was 0.712.

• Korean journal of food and cookery science
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• v.14 no.5
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• pp.541-546
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• 1998

Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.

• Analytical Science and Technology
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• v.24 no.6
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• pp.421-428
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• 2011

In this study, headspace disk type monolithic material sorptive extraction (HS-MMSE) was developed, validated and applied to the analysis of volatile aroma compounds from vanilla perfume by gas chromatography -mass spectrometry (GC/MS). HS-MMSE uses monolithic material (MonoTrap) based on silica bonded with octadecyl silane (ODS) and activated carbon as a sorbent. Aroma compounds was adsorbed onto the MonoTrap in headspace and extracted by only 100 ${\mu}L$ of solvent. Total 12 volatile compounds from vanilla perfume were successfully analyzed using HS-MMSE. The influence of extractive parameters was investigated and optimized, using benzyl acetate, linalyl acetate, vanillin, ethyl vanillin as target compounds. Under the optimum condition, the limit of detection (S/N = 3) and the limit of quantification (S/N = 10) of proposed method for the target compounds were obtained within the range of 8.35~13.76 ng and 27.82~45.88 ng, respectively. The method showed good linearity with correlation coefficient more than 0.9888, satisfactory recovery and reproducibility. These results showed that HS-MMSE using disk type MonoTrap is a new promising technique for the analysis of volatile aroma compounds from vanilla perfume.

• 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.