• Mass Spectrometry Letters
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• 제4권1호
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• pp.18-20
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• 2013

Headspace solid phase micro-extraction gas chromatography/flame ionization detection (HS-SPME-GC/FID) method was compared with headspace gas chromatography/mass selective detection (HS-GC/MS). Organic solvent-spiked urine as well as urine samples from workspace was analyzed under optimal condition of each method. Detection limit of each compound by HS-SPME-GC/FID was $3.4-9.5{\mu}g/L$, which enabled trace analysis of organic solvents in urine. Linear range of each organic solvent was $10-400{\mu}g/L$, with fair correlation coefficient between 0.992 and 0.999. The detection sensitivity was 4 times better than HS-GC/MS in selected ion monitoring (SIM) mode. Accuracy and precision was confirmed using commercial reference material, with accuracy around 90% and precision less than 4.6% of coefficient of variance. Among 48 urine samples from workplace, toluene was detected from 45 samples in the range of $20-324{\mu}g/L$, but no other solvents were found. As a method for trace analysis, SPME HS GC/FID showed high sensitivity for biological monitoring of organic solvent in urine.

• 한국식품조리과학회지
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• 제30권5호
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• pp.596-602
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• 2014

Dutch coffee is extracted in low temperature for a longer time than espresso and drip coffee. This study was conducted to investigate changes in the flavor compounds in Dutch coffee resulting from different extraction times and storage days. The fifty six flavor compounds in Dutch coffee were identified using a headspace mass-spectrometer. Major flavor compounds were 2-furfuryl acetate, 5-methylfurfural, pyridine, furfural, 2-acetylfuran, pyridine, 2-methoxyphenol, furfuryl alcohol and some compounds varied with espresso and drip coffee. It was worthy of notice that more diverse compounds were composed of total flavor in Dutch coffee. There were more kinds of flavor compounds in early extracts than in latter ones. The duration of storage didn't significantly affected the peak area percentage of flavor compounds in Dutch coffee except with 2-furfuryl acetate.

• Bulletin of the Korean Chemical Society
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• 제27권2호
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• pp.231-236
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• 2006

A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 $\mu$L. 60 min extraction time at 25 ${^{\circ}C}$ was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant ($K_{lh}$) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, $\beta$-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

• Mass Spectrometry Letters
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• 제13권4호
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• pp.125-132
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• 2022

There are many types of spring blossoms on the Daedeok campus of Chungnam National University (CNU) at the area of 1,600,000 square meters. As an assignment for the class of Analytical Chemistry I for second-year undergraduate students, 2021, flower petals collected from various floral groups (Korean azalea, Korean forsythia, Dilatata lilac, Lilytree, Lily magnolia, and Prunus yedoensis) were analyzed using headspace extraction coupled to gas chromatography-mass spectrometry (HS-GC-MS) to study the aromatic profiles and fragrance compounds of each sample group. Various types of compounds associated with the aroma profiles were detected, including saturated alcohols and aldehydes (ethanol, 1-hexanol, and nonanal), terpenes (limonene, pinene, and ocimene), and aromatic compounds (benzyl alcohol, benzaldehyde). The different contribution of these compounds for each floral type was visualized using statistical tools and classification models based on principal component analysis with high reliability (R² = 0.824, Q² = 0.616). These results showed that HS-GC-MS with statistical analysis is a powerful method to characterize the volatile aromatic profile of biological specimens.

• 한국식품과학회지
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• 제31권6호
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• pp.1465-1470
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• 1999

충북청원에서 재배되고 있는 애플민트(Mentha rotundifolia(L) Huds)의 향기성분과 특성을 조사하기 위해 SDE, SFE, headspace 추출하여 GC, GC/MS로 동정하였으며 GC-sniffing test로 향기특성을 조사하였다. 그 결과, 총 67개의 화합물이 동정되었으며 SDE 추출물에서는 39개, SFE추출물에서는 42개, headspace 추출물에서는 16개가 동정되었다. 동정된 화합물 중 SDE와 headspace추출물은 terpene화합물이, SFE추출물은 hydrocarbone류가 여러종류로 나타났다. 그러나 SDE와 SFE추출물의 주성분은 piperitenone oxide, germacrene-D, trans sabinene hydrate등으로 유사하였으나 headspace추출물은 3-octanol, 1,8-cineol, camphene, benzeneacetadehyde등으로 다른 경향을 나타내었다. Sniffing test로 향기특성과 강도 및 화합물을 동정한 결과 SDE추출물을 구성하는 주된 향기특성으로는 상큼한 단내와 사과냄새(ethyl 2-methyl butanoate), 단내와 과일내$({\alpha}-thujene)$, 생버섯내(1-octen-3-ol, 3-octanol) 그리고 쓴 약초향$({\delta}-cadidene)$이었다. Headspace 추출물의 주된 향기특성으로는 알코올내, 상큼한 단내와 사과냄새(ethyl 2-methyl butanoate), 화학적이고 불쾌한내 그리고 쓴약초와 풀내(camphene)로 나타났다.

• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1693-1698
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• 2012

A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

• Bulletin of the Korean Chemical Society
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• 제25권2호
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• pp.271-279
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• 2004

The aroma component of Hallabong peel has been characterized by GC-MS with two different extraction techniques: solid-phase trapping solvent extraction (SPTE) and headspace solid-phase microextraction (HSSPME). Aroma components emitted from Hallabong peel were compared with those of other citrus varieties: lemon, orange and grapefruit by SPTE and GC-MS. d-Limonene (96.98%) in Hallabong was the main component, and relatively higher peaks of cis- ${\beta}$-ocimene, valencene and -farnesene were observed. Other volatile aromas, such as sabinene, isothujol and ${\delta}$-elemene were observed as small peaks. Also, principal components analysis was employed to distinguish citrus aromas based on their chromatographic data. For HSSPME, the fiber efficiency was evaluated by comparing the partition coefficient ($K_{gs}$Kgs) between the HS gaseous phase and HS-SPME fiber coating, and the relative concentration factors (CF) of the five characteristic compounds of the four citrus varieties. 50/30 ${\mu}$m DVB/CAR/PDMS fiber was verified as the best choice among the four fibers evaluated for all the samples.

• 한국식품영양과학회지
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• 제35권10호
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• pp.1405-1411
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• 2006

국내에서 유통되는 국내외 브랜드의 extra virgin급과 정제/혼합 올리브유에 잔류된 헥산의 함량을 측정하기 위하여 신속하고 간편한 headspace법을 이용한 전자코(a-FOX 3000, Alpha M.O.S., France)를 이용하여 분석하였으며, head-space-SPME 법을 사용한 GC/MS 분석방법을 이용하여 정량하였다. 전자코 분석결과, 올리브유에 함유된 헥산의 존재 유무 및 농도를 예측할 수 있을 것으로 사료되었으며, 1차로 수거된 국내에 유통 중인 5종의 국내 브랜드 extra virgin급, 10종의 국외브랜드 extra virgin급과 7종의 국내외 브랜드인 혼합/정제 올리브유의 경우 헥산의 잔류 합유량은 잔류되어 있지 않거나, 잔류되어 있다고 하더라도 국내 허용치인 5 ppm 미만으로 예측되었다. 잔류 헥산을 정량하기 위하여 polydimethylsiloxane(PDMS)으로 코팅된 fiber를 사용한 headspace SPME-GC/MS를 사용하였다. 이 때 시료의 head space산출을 위한 최적의 휘발촉진 온도를 선정하기 위하여 각 온도별 검량선 작성한 결과 $R^2$값이 99.99%로 가장 재현성이 높을 것으로 판단되는 $70^{\circ}C$에서 30 min 동안의 휘발촉진과정을 통하여 휘발성분을 fiber에 흡착하였다. 1차로 수집한 총 22개의 올리브유 중 총 6개의 시료에서 헥산이 검출되었고, 2차로 수집한 총 19개의 올리브유에서는 총 2개의 시료에서 헥산이 검출되었으나, 검출된 잔류 헥산의 양은 모두 국내 규정한계농도(5 ppm) 이하인 1 ppm 이하인 것으로 확인되었다.

• 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.

• 한국식품위생안전성학회지
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• 제22권4호
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• pp.243-247
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• 2007

헤드스페이스-기체크로마토그래프/질량분석기를 이용하여 음료류 중 벤젠을 분석하였다. 대상식품은 시중에 유통되는 과실쥬스 2종, 과실음료 6종, 착향탄산음료 11종, 혼합음료 55종, 추출음료 7종, 음료베이스 4종 등 총 85종이었다. 헤드스페이스의 상평형을 위하여 $40^{\circ}C$에서 30분간 교반하였으며 오븐온도는 초기 온도 $60^{\circ}C$에서 5분간 유지 후 $15^{\circ}C$/분의 비율로 $180^{\circ}C$까지 상승하였다. 내부표준물질로는 벤젠-d6을 사용하였다. 선택이온 m/z 51, 77, 78로 확인하였으며 선택이온 m/z 78에 대한 m/z 77의 반응세기비로 재검증하였다. 벤젠의 선택이온 m/z 78과 내부표준물질 벤젠-d6의 선택이온 m/z 84에 대한 피크 면적비로 정량하였다. 회수율은 $91{\sim}101%$이었으며, 정량한계는 $1{\mu}g/kg$이었다. 벤젠의 평균검출수준은 과실음료의 경우 $5{\mu}g/kg$, 착향탄산음료의 경우 $2{\mu}g/kg$, 혼합음료의 경우 $7{\mu}g/kg$, 추출음료의 경우 $7{\mu}g/kg$이었다.