• Applied Biological Chemistry
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• 제40권2호
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• pp.144-147
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• 1997

식물체의 향기성분을 분리하는데 사용되는 몇가지 방법을 비교하기 위해서 headspace(purge & trap)법, simultaneous distillation extraction(SDE)법, steam distillation법, 용매추출법 등으로 분리된 휘발성 성분의 조성차이를 분석하여 각각의 사용된 방법들의 특징을 비교하였다. 휘발성 성분 분석시료로는 Anise(Pimpinella anisum L.)씨앗을 사용하였으며 분리된 휘발성분중 GC/MSD를 이용하여 43종의 성분을 확인하였다. Headspace (purge & trap)법에서는 휘발성이 강한 2-butanol, pentanal, 3-hexen-1-ol 등과 같은 alcohol류 및 aldehyde류 성분들을 주요성분으로 확인할 수 있었으며, 용매추출에서는 비점이 높은 성분들인 myristic acid, oleic acid 등의 acid류 성분들과 ethyl hexadecanoate, ethyl octadecanoate 등과 같은 ester 화합물들이 주요성분으로 확인되었다. SDE법과 steam distillation법에서 추출된 성분의 조성은 유사하였으며 terpene 화합물들이 주요성분으로 확인되었다. Anise의 주성분인 anethole은 SDE법, headspace(purge & trap)법으로 추출하였을때 가장 많이 추출되었다.

• 분석과학
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• 제9권4호
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• pp.399-405
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• 1996

참기름 중의 향기성분을 연속수증기증류법(SDE)과 동적헤드스페이스법(DHS)으로 포집하여 GC와 GC-MSD로 동정하였다. SDE로 분석하였을 때 alcohol 6종, aldehyde 6종, ketone 및 acid류 5종, furan 및 phenol류 4종, pyrazine 화합물 12종, pyridine 및 thiazole류 4종, 기타 9종으로 총 46종이 확인되었다. DHS로 분석한 경우 alcohol 3종, aldehyde 6종, ketone, furan 및 phenol류 6종, pyrazine류 12종, pyridine 및 thiazole 4종, 기타 5종으로 모두 36종이 확인되었다. 대부분의 화합물이 SDE법에서 분리된 것이었으나 1-hexanol, pentanal, dimethylsulfide등은 DHS법에 의해서만 분리되었다.

• 한국연초학회지
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• 제35권1호
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• pp.7-12
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• 2013

A Solid-phase micro extraction(SPME) was evaluated as a tool for headspace sampling of tobacco samples. Several experimental parameters (sampling temperature, pH, and type of SPME fibers) were optimized to improve sampling efficiency in two aspects ; maximum adsorption and selective adsorption of volatile organic acids onto SPME fibers. Among four types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate), Car/PDMS (Carboxen/Polydimethylsiioxane) and PDMS/DVB(Polydimethylsiioxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency. A variety of tobacco samples such as flue cured, burley and oriental were used in this study. The effect of these parameters was often dominated by the physical and chemical nature (volatility, polarity) of target compounds. This method allowed us to make important improvements in selectivity and sensitivity. The Car/PDMS fiber was shown to be the most efficient at extracting the 10 selected volatile organic acids. The parameters were optimized: $80^{\circ}C$ adsorption temperature, 30 min of adsorption time, $240^{\circ}C$ desorption temperature, 1 min of adsorption time.

• Bulletin of the Korean Chemical Society
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• 제33권12호
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• pp.3963-3970
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• 2012

Headspace (HS) and headspace solid-phase microextraction (HS-SPME) were studied for extracting volatile organic compounds (VOCs) from whole blood, with chemical and instrumental variables being optimized for maximum sensitivity: incubation at $60^{\circ}C$, equilibration for 30 min, pH 11, and 2 mL injection volume. Both techniques provided accurate analyses, with detection limits of 0.05-0.1 ng $mL^{-1}$ and 0.05-0.5 ng $mL^{-1}$. HS showed better sensitivity, reproducibility, and analysis times than HS-SPME. Overall levels of chloroform in whole blood were found to be 0.05-5.84 ng $mL^{-1}$; detected levels of benzene were 0.05-2.20 ng $mL^{-1}$.

• 한국식품영양학회지
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• 제13권2호
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• pp.118-124
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• 2000

Lipoxygenase(LOX) in soybeans is responsible for beany flavors which limit the wide utilization of soybeans to foods. This study was conducted to analyze beany flavor compounds of the normal Hwagkeumkong and LOX-deficient soybean cultivars, Jinpumkong which lacks L-2, L-3, and Jinpumkong 2 which lacks all L-1, L-2, L-3. Using the combination of dynamic headspace sampling and gas chromatography-mass selective detector(DHS-GC-MSD) for analyzing volatile compounds, hexanal and hexanol were identified in whole soy flour of all three soybena cultivars. Hwangkeumkong had more volatile compounds than Jinpumkong and Jinpumkong 2 in defatted soy flour. Hexanal and acetic acid were identified in soy milk of all three soybean cultivars but Hwangkeumkong had more volatile compounds than Jinpumkong 2. From the analysis with a static headspace sampling(SHS) and GC-MSD the major compounds were hexanal, acetic acid, 1-hexanol, and 1-octen-3-ol. The content of acetic acid was similar among three cultivars. But contents of hexanal and pentanal in Jinpumkong 2 were less than that of Jinpumkong and Hwangkeumkong. Using GC-FID, Jinpumkong 2 had less contents of hexanal and pentanol than Hwangkeumkong in whole soy flour and defatted soy flour. In this study, LOX-deficient soybean cultivars showed less hexanal, pentanol and other compounds than the normal Hwangkeumkong. However quite amount of beany flavor compounds were identified in Jinpumkong and Jinpumkong 2. So further studies are required to characterize LOX isozymes, to understand the mechanisms of beany flavors production, and to develop some other methods for removing beany flavor.

• Bulletin of the Korean Chemical Society
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• 제30권11호
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• pp.2675-2679
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• 2009

This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

• Applied Biological Chemistry
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• 제40권6호
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• pp.536-540
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• 1997

고품질 당근을 육성하기 위한 연구의 일환으로 당근의 휘발성 terpenoids를 GC 분석으로 측정하였다. 여러가지 휘발성 terpenoids 표준물질을 DHS(direct headspace sampling)방법으로 검출한 결과 ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, ${\alpha}-terpinene$, limonene, ${\gamma}-terpinene$, terpinolene 의 7가지 성분이 명확히 분리되었으나, ${\alpha}-phellandrene$은 ${\beta}-myrcene$으로부터 분리되지 않았다. 또한 terpinen-4-ol, bornyl acetate, ${\alpha}-bisbolol$ 등 비등점이 높은 물질은 검출되지 않았다. 검출된 7가지 terpenoids 성분의 표준곡선은 결정계수$(r^2)$가 전부 0.99 이상으로서 고도로 유의한 표준곡선이었다. DHS 방법을 통한 본실험의 재현성을 측정한 결과, ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, limonene, ${\gamma}-terpinene$, terpinolene, total terpenoids의 변이 계수(C.V.)가 각각 6.8, 6.8, 8.4, 7.1, 3.8, 10.1, 7.1%로 $3.8{\sim}10.1%$의 범위를 나타내었다. 세계적으로 많이 재배되는 당근 65품종에 대한 ${\alpha}-pinene$, ${\beta}-pinene$, ${\beta}-myrcene$, ${\alpha}-terpinene$, limonene, ${\gamma}-terpinene$, terpinolene, total terpenoids를 측정한 결과, 각각 $0.28{\sim}2.48\;ppm$, $0.35{\sim}1.87\;ppm$, $0.56{\sim}1.51\;ppm$, 0 ppm, $0.59{\sim}1.84\;ppm$, $0.87{\sim}3.33\;ppm$, $5.15{\sim}35.81\;ppm$, $9.07{\sim}42.30\;ppm$으로서 품종에 따라 상당한 차이를 보였다. Total terpenoids 의 경우 65품종 중 5품종(7.7%)이 10 ppm미만이고, 15품종(23.1%)이 $10{\sim}11.99\;ppm$, 14품종(21.5%)이 $12{\sim}13.99\;ppm$, 9품종(13.8%)이 $14{\sim}15.99\;ppm$, 10품종(15.4%)이 $16{\sim}17.99\;ppm$, 4품종(6.2%)이 $18{\sim}19.99\;ppm$, 5품종(7.7%)이 $20{\sim}29.99\;ppm$, 3품종(4.6%)이 30 ppm 이상이었다. 전반적으로 일본에서 육성된 품종이 구미에서 육성되어 보급되고 있는 품종들에 비해 total terpenoids 함량이 낮은 편이었다.

• 한국식품과학회지
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• 제24권2호
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• pp.171-176
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• 1992

더덕(Codonopsis lanceolata)의 휘발성 향기성분을 분석하기 위해 gas co-distillation(GCD), solvent extraction/fractionation(SLF), headspace sampling(HSS) 방법을 사용하여 향기성분을 분리농축하고 분석 비교한 결과 SEF와 HSS 방법으로 얻은 농축물들의 향이 원래의 더덕향과 가장 유사했으며 gas chromatogram들의 양상도 비슷했으나 peak들의 크기에 있어서 차이를 보였다. SEF 농축물에서는 달콤한 향을 기리고 HSS 농축물에서는 풋내를 비교적 강하게 느낄 수 있었으나 GCD 농축물의 경우 일정 증류시간이 지나면 한악취를 느낄 수 있었다. SEF와 HSS 방법은 GCD에 비해서 적은 조작 단계로 손쉽게 빠른 시간내에 분리 농축이 가능했다. 농축한 향기성분은 GC-MS와 극성이 다른 두 column을 사용한 GC-RI system을 이용하여 확인하였다. 특히 GC-RI는 isomer의 확인에 효과적이었으며 극성 FFAP column은 극성 화합물의 확인에 보다 적합했다. 35가지의 향기성분들을 동정하였는데 그중 24개의 성분들은 simultaneous distillation extraction 농축물에서는$^{(5)}$ 확인되지 않았던 향기성분들이다. 화인된 성분들중 trans-2-hexenal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, hexanol은 더덕의 풋내를, 1-octen-3-ol은 신선한 풍미를 그리고 amyl propionate를 비롯한 다수의 에스터 화합물 등은 더덕 특유의 달콤한 향에 복합적으로 작용할 것으로 추정된다.

• Bulletin of the Korean Chemical Society
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• 제34권1호
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• pp.139-142
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• 2013

A study was carried out to evaluate the solid phase micro-extraction (SPME) for formaldehyde emission analysis of uncoated plywood. In SPME, formaldehyde was on-fiber derivatized through headspace extraction and analyzed by gas chromatography coupled with mass spectrometry (GC/MS). The SPME was compared with desiccators (DC-JAS 233), small-scale chamber (SSC-ASTM D6007) and liquid-liquid extraction (LLE-EPA 556) methods which were performed in accordance with their respective standards. Compared to SSC (RSD 4.3%) and LLE (RSD 5.0%), the SPME method showed better repeatability (RSD 1.8%) and not much difference from DC (RSD 1.4%). The SPME has proven to be highly precise (at 95% confidence level) with better recovery (REC 102%). Validation of the SPME method for formaldehyde quantitative analysis was evidenced. In addition, the SPME by air sampling directly from plywood specimens (SPME-W) correlated best with DC ($r^2$ = 0.983), followed by LLE ($r^2$ = 0.950) and SSC ($r^2$ = 0.935).

• Elastomers and Composites
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• 제54권3호
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• pp.188-200
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• 2019

Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.