• Bulletin of the Korean Chemical Society
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• 제34권9호
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• pp.2691-2696
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• 2013

The electronic cigarette (E-cigarette) is a battery-powered device that aerosolizes nicotine so that it is readily delivered into the respiratory tract. The analytical data regarding the substances present in E-cigarettes are very limited. The aim of this study was to measure the concentration of aldehydes-formaldehyde (FA), acetaldehyde (AA) and, acrolein (AL)-in 225 replacement liquid brands from 17 E-cigarette shops sold in the Republic of Korea by headspace solid-phase micro extraction and gas chromatography-mass spectrometry (HS-SPME GC-MS). The concentration range of FA and AA was 0.02-10.09 mg/L (mean = 2.16 mg/L, detected in 207 of 225 samples) and 0.10-15.63 mg/L (mean = 4.98 mg/L, detected in all samples), respectively. AL was not detected in any of 225 replacement liquids. FA and AA were originally present in almost all replacement liquids of electronic cigarettes.

• Journal of the Korean Wood Science and Technology
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• 제45권6호
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• pp.682-688
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• 2017

Fresh japanese anise (Illicium anisatum L.) tree leaves were collected and ground after drying. The essential oils of the leaves were analyzed by gas chromatography-mass spectrometry (GC-MS) using headspace (HS) and solid phase-microextra (SPME) methods. Volatile components of the leaves were identified 21 and 65 components in HS and SPME, respectively. The main components of the essential oils obtained by HS method were eucalyptol (36.7%), (+)-sabinene (15.61%), ${\delta}$-3-carene (6.87%), ${\alpha}$-pinene (6.07%), ${\gamma}$-terpinen (5.72%), ${\alpha}$-limonene (5.26%), ${\beta}$-myrcene (4.13%), ${\alpha}$-terpinene (4.04%) and ${\beta}$-pinene (3.73%). The other components were less than 3.5%. SPME method also showed that eucalyptol (17.88%) was main. The other were 5-allyl-1-methoxy-2 (13.29%), caryophyllene (6.09%), (+)-sabinene (5.60%), ${\alpha}$-ocimene (4.89%) and ${\beta}$-myrcene (3.73%), and the rest were less amounts than 3.5%. This work indicated that many more volatile components were isolated, comparing to the previous literature data and that SPME method was much more effective than HS method in the analysis of the volatile components.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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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.

• 분석과학
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• 제13권1호
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• pp.72-80
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• 2000

헤드스페이스/가스크로마토그래프/질량분석계(HS/GC/MS)을 이용하여 환경 시료 중 폐기물 시료인 슬러지 중의 휘발성 유기화합물을 분석하였다. 본 연구에서는 헤드스페이스를 이용한 휘발성 물질의 분석에서 염(salt)의 첨가 유무, 평형온도 및 평형시간 등이 미치는 영향을 파악하기 위해서 수행되었다. NaCl을 첨가한 경우와 첨가하시 않은 경우 이들 분석물질의 회수율 변화는 NaCl을 넣었을 때 1,2-dibromo-3-chloropropane이 2.61배로 가장 큰 회수율의 변화를 보였으며, trlchlorofluoromethane이 1.07배로 가장 적은 변화를 나타내었다. 또한, 평형온도는 $80^{\circ}C$에서 $90^{\circ}C$(30분)로 증가됨에 따라 피이크의 면적이 크게 증가한 것으로 나타났으며, 평형도달 시간은 30분($85^{\circ}C$)이 최적 조건으로 조사되었다. 또한, 55종의 분석대상물질의 재현성도 매우 높게 나타나, 이 방법을 이용한 폐기물 시료중의 휘발성 유기화합물의 분석이 가능하리라 판단되어진다.

• 상하수도학회지
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• 제18권5호
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• pp.628-637
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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 disinfection by-products (DBPs) such as haloacetonitriles (HANs), trihalomethanes (THMs), haloacetic acids (HAAs). In this study, headspace-solid phase microextraction (HS- SPME) technique was applied for the analysis of HANs in drinking water. The effects of experimental parameters such as selection of SPME fiber, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and detection limits were also evaluated. The $50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were the optimal experimental conditions for the analysis of HANs. The correlation coefficients ($r^2$) for HANs was 0.9979~0.9991, respectively. The relative standard deviations (%RSD) for HANs was 2.3~7.6%, respectively. Detection limits (LDs) for HANs was $0.01{\sim}0.5{\mu}g/L$, respectively.

• 분석과학
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• 제30권2호
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• pp.68-74
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• 2017

The volatile components in 'Fuji' apple were effectively determined by a headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 48 volatile components were identified and tentatively characterized based on National Institute of Standards and Technology (NIST) MS spectra library and the Kovats GC retention index I (RI). The harvested Fuji apples were divided into two groups: 1-methylcyclopropene (1-MCP) treated and non-treated (control) samples for finding important indicators between two groups. The major volatile components of both apples were 2-methylbutyl acetate, hexyl acetate, butyl 2-methylbutanoate, hexyl butanoate, hexyl 2-methylbutanoate, hexyl hexanoate and farnesene. No significant differences of these major compounds between 1-MCP treated and non-treated apples were observed during 1 month storage. Interestingly, the amount of off-flavors, including 1-butanol and butyl butanoate, in 1-MCP treated apples decreased over 5 months, and then increased after 7 months. However, non-treated apples did not show significant changes for off-flavors during 7 month storage (p<0.05). The non-treated apples also contained the higher levels of two off-flavors than 1-MCP treated apples. These two compounds, 1-butanol and butyl butanoate, can be used as quality indicators for the quality evaluation of Fuji apple.

• Journal of Microbiology and Biotechnology
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• 제31권1호
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• pp.70-78
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• 2021

Identifying the extracellular metabolites of microorganisms in fresh vegetables is industrially useful for assessing the quality of processed foods. Pectobacterium carotovorum subsp. carotovorum (PCC) is a plant pathogenic bacterium that causes soft rot disease in cabbages. This microbial species in plant tissues can emit specific volatile molecules with odors that are characteristic of the host cell tissues and PCC species. In this study, we used headspace solid-phase microextraction followed by gas chromatography coupled with mass spectrometry (HS-SPME-GC-MS) to identify volatile compounds (VCs) in PCC-inoculated cabbage at different storage temperatures. HS-SPME-GC-MS allowed for recognition of extracellular metabolites in PCC-infected cabbages by identifying specific volatile metabolic markers. We identified 4-ethyl-5-methylthiazole and 3-butenyl isothiocyanate as markers of fresh cabbages, whereas 2,3-butanediol and ethyl acetate were identified as markers of soft rot in PCC-infected cabbages. These analytical results demonstrate a suitable approach for establishing non-destructive plant pathogen-diagnosis techniques as alternatives to standard methods, within the framework of developing rapid and efficient analytical techniques for monitoring plant-borne bacterial pathogens. Moreover, our techniques could have promising applications in managing the freshness and quality control of cabbages.

• 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.

• 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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• 제29권5호
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• pp.242-247
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• 2016

본 연구는 물휴지 중 메탄올 정량법을 확립 및 밸리데이션을 수행하고, 확립된 시험법을 인체세정용 물휴지에 적용하여 검증하는 것을 목적으로 하였다. 물휴지 중 메탄올 정량시험은 헤드스페이스/가스크로마토그래피/불꽃이온화검출기법(HS/GC/FID)을 사용하였고, ‘의약품 등 시험방법 밸리데이션에 대한 가이드라인’에 따라 밸리데이션을 수행하였다. 확립된 시험법에서 메탄올의 정량범위는 3~40 μg/mL로 나타났으며, 상관계수(R²) 0.999 이상의 직선성과 우수한 선택성을 나타내었고, 검출한계와 정량한계는 각각 0.36와 1.17 μg/mL로 나타났다. 검출범위 내 농도별 회수율을 시험한 결과는 100.67~110.17%를 나타났다. 정밀성시험 결과 메탄올 검출량의 상대표준편차(RSD %)는 1.83%로 2 % 이내의 결과를 나타났다. 물휴지 중 메탄올 시험법을 유통 중인 물휴지 20개 제품에 적용하여 검출량을 분석한 결과 20개 제품에서 0.00017 %~ 0.00156%로 나타나 검출허용한도 기준 내 적합한 것을 확인하였다.