• Journal of Applied Biological Chemistry
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• v.49 no.4
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• pp.180-185
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• 2006

Two different extraction procedures, SDE and SPME, were employed to determine a comprehensive and efficient fragrance profile of Korean Rosa hybrida. Both extraction methods could compensate for each other, covering compounds with diverse boiling point, polarities, and chemical properties. A total of 46 compounds were identified in Mi-hyang. The identified compounds were composed of 17 alcohols, 14 carbonyls, 7 aliphatic hydrocarbons, 2 terpene hydrocarbons, 4 benzenes, 1 ester, and 1 miscellaneous compound. Quantitatively, carbonyls($12.96{\sim}21.79%$ in essential oils of SDE and $2.89{\sim}8.44%$ in SPME headspace) and alcohols($7.98{\sim}11.73%$ in essential oils of SDE and $3.39{\sim}17.35%$ in SPME headspace) were dominant in Mi-hyang's volatiles.

• 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.

• 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.

• 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.

• 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.

• 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.

• Journal of Life Science
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• v.28 no.12
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• pp.1523-1528
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• 2018

This study investigated the chemical composition of four Korean cultivated Chrysanthemum indicum L. (Gamguk 1 ho, Gamguk 2 ho, Gamguk 3 ho, and Wonhyang) which are used in the food and fragrance industries to identify their volatile flavor compounds. These compounds were analyzed using headspace GC-MS from plant samples cultivated in the same region of Korea (Sancheong-gun, Gyeongsangnam-do). A total of 23 compounds were identified, eight of which were common across the four cultivars. The major flavor components in the three Gamguk plants were identified as 3-carene, camphene, ${\beta}$-phellandrene, eucalyptol and (+)-camphor. Eleven compounds, including (+)-camphor at 31.40%, were identified in Gamguk 1 ho. Gamguk 2 ho was found to contain 12 flavor compounds, predominant of which was camphene at 25.60%. Thirteen compounds including (+)-camphor (26.88%) were identified in Gamguk 3 ho, while 17 were detected in the Wonhyang cultivar, including trans-piperitol (47.33%), sabinene, and ${\gamma}$-terpinyl acetate. These results indicate differences in the type and ratio of functional volatile flavor ingredients in Chrysanthemum indicum L. cultivars which is highly valuable as material for fragrance product development.

• 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.

• Journal of the Korean Society for Marine Environment & Energy
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• v.17 no.1
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• pp.27-35
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• 2014

The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.