• Bulletin of the Korean Chemical Society
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• v.28 no.12
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• pp.2389-2395
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• 2007

Headspace solid phase trapping solvent extraction (HS-SPTE) and GC-MS was applied for the characterization of volatile flavors from fennel, anise seed, star-anise, dill seed, fennel bean, and Ricard aperitif liquor. Tenax was used for HS-SPTE adsorption material. Recoveries, precision, linear dynamic ranges, and the limit of detection in the analytical method were validated. There were some similarities and distinct differences between fennel-like samples. The Korean and the Chinese fennels contained trans-anethole, (+)-limonene, anisealdehyde, methyl chavicol as major components. The volatile aroma components from star anise were characterised by rich trans-anethole, (+)-limonene, methyl chavicol, and anisaldehyde. Additionally, principal component analysis (PCA) has been used for characterizing or classifying eight different fennel-like samples according to origin or other features. A quite different pattern of dill seed was found due to the presence of apiol (dill).

• Korean Journal of Food Science and Technology
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• v.24 no.2
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• pp.171-176
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• 1992

Volatile flavor components of Codonopsis lanceolata were extracted by gas co-distillation (GCD), solvent extraction/fractionation (SEF), and headspace sampling (HSS) methods. The extracts were analyzed by dual-capillary gas chromatography-retention index (GC-RI) and gas chromatography-mass spectrometry(GC-MS). The two extracts prepared by SEF and HSS gave more similar fragrance to the Codonopsis lanceolata than the GCD extract. The GC profiles of the SEF and HSS extracts were similar to each other except for differences in peak areas. The extract prepared by SEF gave a sweet note while the extract prepared by HSS gave a green note. The GCD extract began to give a burnt note of herb medicine with prolonged distillation. Rapid extraction of flavor components from Codonopsis lanceolata was possible in several short steps by SEF and HSS methods compared to GCD. GC-MS and GC-RI were used for peak identification. GC-RI was more effective for identification of isomers, and polar FFAP column was more suitable for identification of polar compounds. From Codonopsis lanceolata we identified 35 volatile flavor constituents, 24 of which have not been previously reported by simultaneous distillation extraction method $^{(5)}$. trans-2-Hexanal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, and hexanol were considered key components of the green note and 1-octen-3-ol, the component of the fresh note. Esters, including amyl propionate, seem to be responsible for the sweet note particular to Codonopsis lanceolata.

• Analytical Science and Technology
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• v.27 no.1
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• pp.22-26
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• 2014

1,4-Dioxane was classified as a Group 2B carcinogen by the International Agency for Research on Cancer. The compound was measured in surface water with a headspace gas chromatographic mass spectrometric detection. A 5 mL water sample was placed in a 10 mL headspace vial and saturated with NaCl, and the solution was spiked with 1,4-dioxane-d8 as an internal standard and sealed with a cap. Water samples were collected from twenty-two basins of Gum-River on June and September 2012, respectively. As a result, 1,4-dioxane was detected in the concentration range of $0.49-43.0{\mu}g/L$ (mean $2.0{\mu}g/L$) in the frequency of about 30% in surface water samples.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.1
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• pp.26-31
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• 2002

Volatile compounds from three parts of needles, sprouts and twigs in Pinus densiflora were extracted by solid phase microextraction (SPME) and dynamic headspace analysis (DHA). separated by gas chromatography, and identified by using mass selective detecter and Kovat's retention index. The amounts of monoterpenes isolated by SPME and DHA were 66.7% and 14.3% in needles, 90.6% and 0.7% in sprouts, and 90.6% and 1.2% in twings, respectively. The amounts of sesquiterpenes detected only by SPME were 25.8% in needles, 4.4% in twings and 1.5% in sprouts. And the amounts of oxygenated terpenes isolated by SPME and DHA were 4.7% and 79.0% in sprouts, 3.7% and 70.4% in twigs, and 1.0% and 50.7% in needles, respectively. The kinds of volatile compounds isolated by SPME were similar to those by solvent extraction, but the number of compounds identified to hate a boiling point below 5$0^{\circ}C$ by UHA was larger than that of SPME.

• 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.

• Bulletin of the Korean Chemical Society
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• v.30 no.1
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• pp.35-42
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• 2009

Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

• The Korean Journal of Food And Nutrition
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• v.10 no.1
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• pp.25-30
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• 1997

Volatile components of green tea were isolated by purge and trap headspace method and were analyzed by GC and GC/MSD. And ten headspace volatiles were compared with volatiles isolated by simultaneous distillation-extraction(SDE) method. A total of 99 components were identified in the green tea volatile components, from which 88 components were identified in the headspace volatiles, contained 20 alcohols, 30 hydrocarbons, 21 aldehydes, 10 ketones, 2 acids and 5 miscellaneous components. The major components were low boiling components, such as methyl butanal(3.1%), 1-penten-3-ol(5.48%), 2-penten-1-ol(2.89%), hexanal(5.77%), heptanal(1.90%), and ere 2,4-eptadienal(4.28%), linalool(2.27%), 2,6-dimethyl cyclohexanol(2.57%), $\alpha$-pinene(1.52%), caryophyllene(1.70%), and carbonyl compounds, such as $\alpha$-ionone(2.62%), $\beta$-ionone(2.98%), $\beta$-cyclocitral(2.0%). On the other hand SDE volatiles, from which 64 components were identified, contained 16 alcohols, 16 ydrocarbons, 15 aldehydes, 10 ketones, 3 acids and 4 miscellaneous components. The major components were alcohols, such as, benzyl alcohol(3.79%), linalool(9.52%), terpineol(2.16%), geraniol(2.75%), nerolidol(6.50%), ketones, such as $\alpha$-ionone(1.77%), $\beta$-ionone(4.80%), geranyl acetone(1.82%) and acids, such as hexanoic acid(1.45%), nonanoic acid(1.11%).

• 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.

• Korean Journal of Medicinal Crop Science
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• v.8 no.1
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• pp.49-57
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• 2000

To understand the effects of drying conditions on changes of volatile compounds in fruits of Schizandra chinensis, we analyzed SDE (steam distillation and extraction) extract and Headspace vapor of fresh and dried samples using GC/MS (Gas chromatograph/Mass spectrometer). Contents of essential oils from samples with different drying conditions were 0.58% in fresh ones, 0.60% in freeze dried ones, and 0.30% in hot-air dried ones. In SDE extract, major volatile compounds in fresh samples were terpinen-4-ol(9.01%), ${\gamma}-terpinene(7.02%),\;{\beta}-myrcene(7.55%)$, unidentified sesquiterpenes(28.48%), showing almost the same composition as that in freeze-dried ones, but those in hot-air dried samples at $60^{\circ}C$ were ${\gamma}-terpinene(5.40%),\;{\alpha}-elemene(8.28%)$, unidentified sesquiterpenes(50.38%), indicating the chemical changes during drying procedure. In Headspace vapor, major compounds in fresh samples were ${\beta}-myrcene(22.05%),\;{\gamma}-terpinene(9.47%),\;{\alpha}-pinene(8.91%)$, sabinene(8.48%), which were different from those in SDE extract. In chemical compositions of volatile compounds in dried samples, ${\beta}-myrcene,\;{\alpha}-terpinene$ decreased in the order of freeze-drying > hot-air drying at $60^{\circ}C$ > hot-air drying at $60^{\circ}C$, and ${\alpha}-ylangene,\;{\alpha}-pinene$, camphene increased in the reverse order of the former. We observed the changes of the contents and compositions of essential oils compounds during drying procedure, especially a decrease in monoterpenes and alcohols and an increase in sesquiterpenes with relatively weak volatility.

• Journal of the Korean GEO-environmental Society
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• v.11 no.5
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• pp.61-67
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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 chlorinated solvents (PCE and TCE) and these by-products (cis-DCE, VC, and Ethylene). 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 50mL, sodium chloride (NaCl) concentration of 25% combined with magnetic stirring were selected in optimal experimental conditions for analysis of chlorinated solvents and these by-products. The general affinity of analytes to CAR/PDMS fiber was high in the order PCE>TCE>cis-DCE>VC>Ethylene. The linearity of $R^2$ for chlorinated solvents and these by-products was from 0.912 to 0.999 when analyte concentrations range from $10{\mu}g/L$ to $500{\mu}g/L$, respectively. The relative standard deviation (% RSD) were from 2.1% to 3.6% for concentration of $500{\mu}g/L$ (n=5), respectively. Finally, the limited of detection (LOD) observed in our study for chlorinated solvents and these by-products were from $0.5{\mu}g/L$ to $10{\mu}g/L$, respectively.