• 한국식품과학회지
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• 제33권1호
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• pp.153-156
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• 2001

2단계 발효로 제조한 감식초를 static headspace-GC법과 SPME-GC법으로 휘발성 성분을 각각 포집 분석하여 상호간의 특성에 대해 조사하였다. 감식초의 휘발성 성분 포집조건은 $80^{\circ}C$에서 20분간으로 설정하였으며, 감식초 휘발성 성분의 total FID response는 CW/DVB fiber를 이용한 SPME법에서 total peak area $18.18{\times}10^6$로, static headspace-GC법의 total peak area $1.35{\times}10^6$보다 현저하게 높았다. 감식초의 주된 휘발성 성분으로 acetic acid, ethyl acetate, 3-hydroxy-2-butanone, ethanol, phenethyl alcohol 등이 확인되었으며, static headspace-GC법에서는 acid류 3종, aldehyde류 3종, alcohol류 5종, ester류 8종 및 ketone류 1종이 확인되었다. SPME-GC법에서는 acid류 6종, aldehyde류 7종, alcohol류 6종, ester류 9종, hydrocarbone류 2종, ketone류 1종, 기타 3종으로, 총 34종의 휘발성 성분이 확인되었으며, benzaldehyde, phenethylacetate, phenethylalcohol 등의 비율이 headspace-GC법에 비해 높았다.

• 한국식품과학회지
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• 제38권6호
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• pp.738-741
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• 2006

본 실험에서는 시판중인 우유 4종을 대상으로 static headspace, purge and trap 및 SPME의 세 가지 향기성분 추출방법을 이용하여, GC/MS로 각각의 향기성분을 분석하였다. Purge and trap법을 이용한 분석법으로 가장 많은 종류의 성분을 분석할 수 있었으며, 향기성분의 추출효율이 가장 좋았다. SPME법은 간단한 장비로 신속하게 향기성분을 포집할 수 있는 장점이 있으며, 추출 효율 또한 뛰어나 효율적인 향기성분 분석방법으로 이용이 가능하였다. 4종의 시판우유 중에서 검출된 향기성분은 대체적으로 큰 차이를 나타내지 않았으나, 다소의 양적차이를 나타내었다. 검출 된 성분은 주로 acetone, 2-butanone, 2-pentanone, 2-heptanone, 2-nonanone 등의 케톤류, pentanal, 2-methylbutanal, hexanal, benzaldehyde 등의 알데하이류 및 dimethyl sulfide 등의 황화합물류로써, 우유의 주요 이취성분들이었다.

• 한국식품과학회지
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• 제28권6호
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• pp.1177-1179
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• 1996

식품포장재에 함유되어있는 톨루엔 및 잔류용제를 용출분석하는 방법으로 headspace gas chromatography (static headspace method)를 이용하였다. 5종(methanol, isopropyl alcohol, ethyl acetate, methyl ethyl ketone, toluene)의 표준용제에 대한 머무름시간과 상대표준편차를 검토해 본 결과, 이상적인 머무름시간의 상대표준편차라 할 수 있는 0.15% 이하로 양호하였으며 재현성도 우수하였다. 인쇄된 포장재를 분석한 결과. 주로 methanol, toluene, methyl ethyl ketone이 검출되었고, methanol은 불검출${\sim}0.939\;mg/m^2$, toluene은 불검출${\sim}1.403{\;}mg/m^2$, methyl ethyl ketone은 불검출${\sim}0.932\;mg/m^2$ 함유 되어있는 것으로 나타났으며, 총 잔류 용제는 불검출${\sim}2.433{\;}mg/m^2$ 함유되어 있는 것으로 나타났다.

• Food Science and Biotechnology
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• 제14권4호
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• pp.456-460
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• 2005

To enforce the maximum residue limit for residual hexane (0.005 g/kg) in commercially available Korean vegetable oil, convenient and accurate quantification methods were investigated. Using dual surrogate standards, pentane and heptane were dissolved in ethanol, and then added to hexane-tree sunflower oil for setting up the calibration curve. Gas Chromatograph-Flame Ionization Detector with a porous layer open tubular column, indicated good chromatographic separation of hexane from other inhibiting matrix components. The lowest calibration level was $0.5\;{\mu}g/g$, not exceeding a relative standard deviation of 10% (RSD%), and 1.0\;{\mu}g/g$ not exceeding a deviation of 22% RSD% using heptane as an internal standard for the Static headspace analysis by using a headspace auto-sampler and manual injection, respectively. The residual hexane was detected in nine of the samples among 87 vegetable oil samples purchased on the local market.

• Bulletin of the Korean Chemical Society
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• 제35권11호
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• pp.3280-3288
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• 2014

Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method ($r^2$ > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to $200ng\;mL^{-1}$. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

• 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 $mL^{-1}$.

• 한국식품과학회지
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• 제37권5호
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• pp.695-701
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• 2005

각각의 황 함유 화합물의 표준곡선을 그렸을 때, linear range의 범위는 $10^2$부터 $10^4$까지의 범위를 보였다. Dimethyl trisulfide가 가장 작은 limit of detection(LOD) 값과 가장 넓은 linear range $(10^4)$를 보이는 반면, methional은 가장 큰 LOD 값과 가장 좁은 linear range$(10^2)$를 가졌다. 각 황 함유 화학물의 분자구조와 PFPD의 황 함유 화합물 분석 원칙에 영향을 받는 것으로 사료된다. 서로 다른 세 종류의 fiber를 사용시, 미세 고체상 추출법(SPME)을 사용했을 때, CAR/PDMS fiber는 가장 좋은 추출 효율을 보였고, 반대로 PDMS/DVB fiber는 가장 낮은 효율을 나타내었다. SPME 방법을 사용하면, 시료에 포함되어 있는 6개의 황 함유 화합물들 중, 최대 5개까지 분석이 가능하였다. 그러나 본 실험에서 사용하지 않은 황 함유 화합물들도 다수 동정 되었는데, 이렇게 추출과정 중 artifacts로 생성된 황 함유 화합물들은 분석 시 오차를 작용할 수 있다. 고정상 기체추출법(SH)은 SPME와 비교했을 때 더 적은 수의 황 함유 화합물을 감지해냈다. SPME와 비교 시 SH의 추출 효율은 낮았지만, artifact로 생성되는 화합물의 수는 적었다.

• 한국식품과학회지
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• 제25권1호
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• pp.52-56
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• 1993

$148-150^{\circ}C$의 팜유에서 약 1분간 튀겨낸 라면을 라면 $65^{\circ}C$에 저장할 때 생성되는 flavor 화합물들을 Gas Chromatography-Mass Spectrometry을 이용하여 분리, 동정하고 20, 40, $65^{\circ}C$에 저장중인 라면에서 생성되는 flavor 화합물들의 양적변화를 static headspace gas chromatography법에 의하여 측정하였다. 라면은 $65^{\circ}C$에 저장되는 동안 pentane, hexane, butanal, heptane, 1-pentanol, hexanal, octane의 화합물을 생성하였는데 이들은 주로 라면의 linoleic acid와 oleic acid로부터 생성되는 듯하다. 이들 화합물들은 저장온도가 20, 40, $65^{\circ}C$로 증가함에 따라 또한 저장기간이 경과함에 따라 그 양이 증가하는 경향을 보였으며 hexanal이 관능검사와 가장 높은 상관관계를 나타내었다(r=0.87).

• 한국식품위생안전성학회지
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• 제14권1호
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• pp.76-83
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• 1999

Solid phase microextraction (SPME) was used for the determination of 6 standard solvents (methanol, isopropanol, methyl ethyl ketone, ethyl acetate, cyclohexane, toluene) in food packaging materials. SPME method is a solvent-free sample preparation technique in which a fused silica fiber coated with polymeric organic liquid is introduced into the headspace above the sample. SPME method using fiber coated polydimethylisiloxane (PDMS) was compared with static headspace (SHS) method used as a reference. It was found that the optimal adsorption condition using PDMS-SPME method was 2$0^{\circ}C$ for 15 minutes for the standard solvents. Detection limits, linearity, reproducibility and recovery of both SHS and PDMS-SPME methods have been determined using 6 standard solvents. Both methods were characterized by high reproducibility and good linearity. Using SHS methods, the mean recovery of the 6 standard solvents was ranged from 75.5% to 105.8% with a mean relative standard deviation (RSD) of 0.3% to 4.8%. With PDMS-SPME method, the mean recovery of the 6 standard solvents was ranged from 86.7% to 108.3% with a mean RSD of 0.4% to 2.5%. The detection limits of both methods were the same for toluene, cyclohexane and methyl ethyl ketone; those of PDMS-SPME method were higher than those of SHS method for methanol, isopropanol and ethyl acetate. PDMS-SPME fiber shoed excellent adsorption for non-polar solvents such as toluene, while it showed relatively low adsorption for polar solvents such as methanol.

• 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.