• 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.

• 약학회지
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• 제54권6호
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• pp.429-440
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• 2010

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

• Bulletin of the Korean Chemical Society
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• 제30권12호
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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.

• 한국산업보건학회지
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• 제32권2호
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• pp.153-162
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• 2022

Objectives: Fused deposition modeling (FDM) 3D printer which is one of the material extrusion (MEX) technologies is an additive manufacturing (AM) process. 3D printers have been distributed widely in Korea, particularly in school and office, even at home. Several studies have shown that nanoparticles and volatile organic compounds (VOCs) were emitted from an FDM 3D printing process. The objective of this study was to identify types of chemicals possibly emitted from FDM 3D printing materials such as PLA (polylactic acid), ABS (acrylonitrile butadiene styrene), nylon, PETG (polyethylene terephthalate glycol), PVA (polyvinyl alcohol), PC (polycarbonate) filaments. Methods: 19 FDM 3D printing filaments which have been distributed in Korea were selected and analyzed VOCs emitted of 3D printing materials by headspace gas chromatography mass spectrometry (headspace GC-MS). Subsamples were put into a vial and heated up to 200℃ (500 rpm) during 20 minutes before analyzing FDM 3D printing filaments. Results: In the case of PLA filament, lactide and methyl methacrylate, the monomer components of one, were detected, and the volume ratio ranged 27~93%, 0.5~37% respectively. In the case of ABS filaments, styrene (50.5~59.1%), the monomer components of one, was detected. Several VOCs among acetaldehyde, toluene, ethylbenzene, xylene, etc were detected from each FDM 3D printing filaments. Conclusions: Several VOCs, semi-VOCs were emitted from FDM 3D printing filaments in this study and previous studies. Users were possibly exposed to ones so that we strongly believe that we recommend to install the ventilation system such as a local exhaust ventilation (LEV) when they operate the FDM 3D printers in a workplace.

• 한국식품조리과학회지
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• 제14권5호
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• pp.541-546
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• 1998

자생 누룩치의 휘발성 향미성분을 연속수증기증류 장치로 추출한 후 GC, GC/MS로 분석하여 31개의 휘발성 향미성분이 확인되었는데, 탄화수소류가 15종으로 전체 peak area의 64.98%를 차지하였고 알데히드류 4종 9.54%, 케톤류 1종 0.16%, 알코올류 5종 7.65%, 에스테르류 2종 2.06%, 산류 3종 2.0% 및 옥사이드류 1종 2.75%로 이루어져 있었다. 탄화수소류 중 mono-terpenes은 peak area 0.54% 및 sesquiterpenes은 52.11% 를 차치하였다. 누룩치의 주요 휘발성 향미성분은 sesquiterpenes인 (Z)-$\beta$-farnesene, (Z, E)-$\alpha$-farnesene 및 farnesene으로 사료된다. Headspace법에 의하여 신선한 누룩치의 휘발성 향미성분을 포집하여 전자코로 분석한 결과, 알코올류와 같은 극성화합물이 가장 많이 감지되었고 알데히드류, 탄화수소류 순서로 감지되었다. 또한 건조된 누룩치는 신선한 시료와 유사한 향미성분 패턴을 보였으나, 각 sensor의 저항치가 현저히 낮아 건조된 시료의 휘발성 향미성분이 비교적 적음을 확인하였다.

• 한국식품영양학회지
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• 제17권3호
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• pp.260-265
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• 2004

솔잎(Pinus densiflora S.)의 휘발성 성분을 추출시간과 온도를 달리하면서 headspace(purge & trap)-GC/MS로 분석하여 총61개의 휘발성 성분을 확인하였다. 확인된 성분을 관능기별로 분류하여 보면 hydrocarbons 35종, alcohols 16종, carbonyls 4종, ethers 3종, esters 2종, acid 1종으로 나타났다. 솔잎에서 확인된 주요 휘발성 성분으로는 $\alpha$-pinene(1.5～15.7%), $\beta$-pinene(0.4～5.4%), $\beta$-myrcene(13.2～15.6%), $\beta$-phellandrene (12.0～16.0%), cis-3-hexenol(4.0～18.3%), $\beta$-caryophyllene (3.6～6.8%) 등이 확인되었다. 또한 headspace(purge & trap)법에 의해 솔잎의 휘발성 성분 분석시 최적 조건을 검토하기 위해 실온에서 2시간과 20시간동안 추출한 것과 6$0^{\circ}C$에서 2시간과 20시간동안 각각 추출했을 때 실온에서 2시간 추출시 가장 많은 56개의 성분이 확인되었고, 실온에서 2시간 추출시 가장 적은 45개의 성분이 확인되었다. 시험조건에 따른 휘발성분 분석에서 비점이 낮은monoterpenes화합물들은 추출시 초기에 주로 추출되어 지고 alcohols류와 비점이 높은 sesquiterpenes 화합물들은 추출시간을 길게 했을 때 더 많은 성분이 추출된다는 것을 알 수 있었다. 4가지 추출조건을 종합해 볼 때 고비점 휘발성 성분 분석에는 6$0^{\circ}C$에서 20시간 추출이 가장 양호하나, 전반적으로 실온에서 20시간 추출이 가장 적합한 조건인 것으로 나타났다.

• Food Science and Biotechnology
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• 제18권1호
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• pp.66-72
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• 2009

An aqueous ribose-cysteine model system (initial pH 5.6) was conventionally heated to the same browning at varying temperatures ($120-180^{\circ}C$), supercritical carbon dioxide (SC-$CO_2$, 20 MPa) was also applied on the same matrices for same periods at each temperature and about 20% reduction of the absorbance at 420 nm was observed as compared with sole thermal treatment. The headspace volatiles from Maillard reaction mixtures were analyzed by solid-phase microextraction (SPME) in combination with gas chromatography and mass spectrometry (GC-MS), and predominated with sulfur containing compounds, such as thienothiophenes, polysulfur alicyclics, thiols, and disulfides. Reaction temperature exhibited complex effects on volatiles formation and those effects became further complicated by the SC-$CO_2$ treatment. The formation of noncarbonyl polysulfur heterocyclic compounds and thienothiophenes was generally favored at high temperatures. Most volatiles were inhibited in SC-$CO_2$ as compared with thermal treatment alone, however, the well-known meaty aromatic compounds, such as thiols and disulfides, were obviously enhanced.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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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.

• 분석과학
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• 제26권5호
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• pp.326-332
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• 2013

Geosmin과 2-methyl isoborneol (2-MIB)는 먹는물에서 불쾌한 맛과 냄새를 일으키는 대표적인 물질이며, 남조류의 대사산물로 흙 냄새나 곰팡이 냄새를 내는 것으로 알려져 있다. 이들 물질의 최소감지 농도는 수 ng/L 수준으로, 먹는물의 질을 관리하기 위해서는 극미량까지 분석할 수 있는 분석방법이 요구된다. 본 연구에서는 물시료 중의 geosmin과 2-MIB를 headspace-solid phase microextraction (HS-SMPE) 법과 기체크로마토그래프/질량분석기 (gas chromatograph/mass spectrometer, GC/MS)를 이용하여 분석하였다. 방법검출한계는 geosmin과 2-MIB에 대하여 각각 1.072 ng/L, 1.021 ng/L 값을 구할 수 있었으며, 정확도와 정밀도에서도 좋은 결과를 얻을 수 있었다. 최근 낙동강에서는 남조류에 의한 수화현상이 종종 발생하고 있어, 낙동강을 상수원수로 하는 먹는물의 안정성을 확보하기 위하여 geosmin과 2-MIB의 농도를 조사할 필요성이 대두되고 있다. 남조류가 번성한 시기에 낙동강 원수에 대하여 geosmin과 2-MIB의 농도를 조사한 결과, 각각 4~24 ng/L, 6~16 ng/L의 농도로 검출되었다.

• 한국산업보건학회지
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• 제33권1호
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• pp.34-39
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• 2023

Objectives: In this study, the safety of alcohol-based hand sanitizers (ABHSs) for quasi-drugs and cosmetics was investigated by analyzing the ethanol content, which is an active ingredient with a sterilizing effect, and methanol, which is toxic. Methods: Forty-one ABHSs were purchased at large supermarkets and online stores. Ethanol quantification was performed by gas chromatography-flame ionization detector, and methanol quantification was performed by headspace-gas chromatography-mass spectrometry. Results: The ethanol content of ABHS in quasi-drugs was 49.6-67.8%, which was suitable for standard manufacturing procedures for external disinfectants, and the ethanol content of ABHS in cosmetics was 9.1-61.3%. The methanol content of ABHS in quasi-drugs ranged from not detected(N.D.)-131.8 ppm, which was suitable for the methanol detection standard of ethanol raw materials in the Korean Pharmacopoeia. The methanol content of ABHS in cosmetics was 23.4-859.7 ppm, which was suitable for the detection limit of methanol in cosmetics. Conclusions: The ethanol and methanol content of ABHS was judged to be safe. When selecting an ABHS to be used for sterilization, it seems necessary to check the content of ethanol, an active ingredient, and use it according to its intended purpose.