• 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.

• Archives of Pharmacal Research
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• 제23권4호
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• pp.374-380
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• 2000

Propentofylline (PPF, 3-methyl-1-(5-oxohexyl)-7-propylxanthine) has been reported to be a compound for treatment of both vascular dementia and dementia of the Alzheimer type. The short half-life (about 15 min) of PPF at the terminal elimination phase and poor bioavailability after oral administration of PPF to rabbits (Kim et al., 1992) suggest in part that this drug takes the extensive first-pass metabolism in the liver. In addition, the metabolic pathway for PPF remains unclear. The objective of this experiment is to identify urinary metabolites of PPF in rats. For the identification of the metabolites, rat urine was collected after oral administration of 100${m}g/kg$ PPF. PPF metabolite, 3-methyl-1-(5-hydroxyhexyl)-7-propylxanthine, was synthesized and confirmed by gas chromatography/mass spectroscopy (GC/MS) and $^1H$ nuclear magnetic resonance spectroscopy. The urinary metabolites of PPF were extracted with diethyl ether and identified by electron impact and chemical ionization GC/MS. One urinary metabolite was confirmed to be 3-methyl-1-(5-hydroxyhexyl)-7-propylxanthine by synthesized authentic compound. Several metabolites of monohydroxy- and dihydroxy-PPF were identified based on mass fragmentation of both intact and trimethylsilylated derivatives of PPF metabolites and the novel structure of these metabolites is suggested based on mass spectra.

• KSBB Journal
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• 제10권2호
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• pp.126-130
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• 1995

초산발효 중 에탄올 농도를 On-line으로 측정하기 위해 막가스 센서를 개발하였다. 에탄올이 함유된 발효액은 실리콘막을 통해 투과되고 Carrier gas로 사용된 Synthetic air에 의해 운반되어 반도체형 가 스센서에 감지되도록 설계하였다. 이 때 실리콘막의 두께가 O.5mm이고 Carrier gas의 유속이 20ml/mim이었을 때 막가스 센서의 감도가 가장 높았다. 막가스센셔의 저항치는 측정하고자 하는 에탄올 농 도에 따라 변하였고 이 저항치는 전위차로 변환되어 출력되었다. 제작된 막가스센서의 Calibration CUf ve를 작성하였고 실제로 조업 중인 초산 발효조의 발효액 중 에단올 농도의 On-line 측정이 가능하였 으며 이를 Gas chromatography에 의한 분석치와 비교한 결과 에단올 농도가 $0∼70g/\ell$의 범위에서 서로 상관관계를 나타내어 이러한 막가스센서가 초산발효와 같은 여러 생물공정의 모니터링과 제어에 이용이 가능함을 확인하였다.

• Archives of Pharmacal Research
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• 제27권1호
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• pp.25-30
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• 2004

Combinatorial homoserine lactone mixtures and individual products were obtained from the methionine-functionalized resin in solid-phase synthesis. The four-step process consisting of a coupling step of an N-Fmoc-L-methionine, deprotection of N-Fmoc group, N-coupling with a carboxylic acid, and cleavage reaction through a polymer supported strategy is described. Gas chromatography-mass selective detector (GC-MSD) techniques provide the most powerful methods for identifying both the combinatorial mixtures and individual products.

• 한국환경농학회지
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• 제1권1호
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• pp.14-21
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• 1982

N-Methylcarbamate계(系) 농약(農藥)의 잔류분석법(殘留分析法)을 확립(確立)하기 위하여 MIPC, XMC, BPMC, propoxur, carbofuran 및 carbary에 대하여 diazo화(化)에 의한 비색정량(比色定量)과 N-trifiuoroacetyl (TFA)화(化), pentafluorobenzyl ether(PFB)화(化) 및 dinitrophenyl ether (DNP)화(化)에 의한 유도체(誘導體)의 gas chromatography (ECD)法을 비교검토(比較檢討)하였다. 1) N-Methylcarbamate의 diazo화(化)에 의한 최대흡수파장(最大吸收波長)은 MIPC, XMC, BPMC, propoxur, carbofuran이 460 ㎚이었고 carbaryl은 510 ㎚이었다. 2) 비색법(比色法)에 의한 carbamate의 현미(玄米)와 사과중(中) 회수솔(回收率)은 명명(各各) $80{\sim}104%$, $98{\sim}120%$이었고, 50 g의 시료분석시(試料分析時) 최대검출한계(最大檢出限界)는 $0.03{\sim}0.05$ ppm의 범위(範圍)이었다. 3) Gas chromatography에 의한 carbamate의 분석(分析)에서는 DNP$0.01{\sim}0.2$ppm첨가시(添加時) 현미(玄米)에서 $74{\sim}94%$, 수도체(水稻體)에서 $78{\sim}93%$, 사과에서 $82{\sim}99%$의 범위(範圍)이었고 검출한계(檢出限界)는 50g의 시료분석시(試料分析時) TFA 0.01 ppm PFB 0.005ppm, DNP 0.01ppm이었다.

• 한국축산식품학회지
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• 제36권2호
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• pp.206-214
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• 2016

The aim of this study was to evaluate the potential use of fatty acids, triacylglycerols, and cholesterol in the detection of adulterated milk fat. The fatty acid, triacylglycerol, and cholesterol profiles of the mixtures of milk and non-milk fat (adulteration ratios of 10%, 30%, 50%, 70%, and 90%) were analyzed by gas chromatography. The results showed that concentrations of the fatty acids with oleic acid (C18:1n9c) and linoleic acid (C18:2n6c), triglycerides with C52 and C54, and cholesterol detected are proportional to the adulteration ratios remarkably. Oleic acid (C18:1n9c), linoleic acid (C18:2n6c), C52, and C54 were lower in pure milk fat than in adulterated mixtures. In contrast, pure milk has a higher cholesterol concentration than all adulterated mixtures (adulteration concentration in the range 10-90%). Thus, we suggest that oleic acid (C18:1n9c), linoleic acid (C18:2n6c), C52, C54, and cholesterol are suitable indicators and can be used as biomarkers to rapidly detect adulterated milk fat by gas chromatography. This study is expected to provide basic data for adulteration and material usage. Moreover, this new approach can detect the presence of foreign oils and fats in the milk fat of cheese and can find application in related studies.

• 한국식품과학회지
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• 제11권2호
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• pp.126-130
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• 1979

향신료 중(中) 식초와 생강의 생선 비린내 억제효과에 관하여 관능검사를 실시하였으며, gas chromatography에 의해 TMA량(量)을 측정하였다 그 결과(結果)는 다음과 같다. 1 관능검사의 결과, 식초 첨가량이 증가할수록 생선 비린내는 점점 감소되었으나, 고등어 100g당(當) 식초를 16m1이상 첨가했을 때는 신맛이 강하게 느껴졌으며 Texture가 단단해져서 질(質)이 저하되었다. 고등어 100g당(當) 식초 6ml를 첨가한 것은 비린내를 싫어하는 사람에 있어서 좋은 점수를 보여 주었다. 2. 고등어 100g 중(中)에는 $0.4{\sim}0.7{\;}mg$의 TMA이 함유되어 있었다. 3. gas chromatography로 분석해 본 결과(結果), 식초 첨가량이 증가할수록 TMA량(量)은 감소되는 경향이 보여졌다. 4. 생강의 phenolic fraction과 TMA과를 4시간(時間) 동안 반응시켰을 때 TMA량(量)은 67.5%로 감소되었다.

• KSBB Journal
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• 제30권4호
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• pp.141-147
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• 2015

The convenient determination of methylsulfonylmethane (MSM) for a commercially available dietary supplement was developed using gas chromatography (GC)-flame ionization detector (FID). Chromatography was performed on a capillary column ($0.32mm\;I.D{\times}30m$, $0.25{\mu}m$) coated with dimethylpolysiloxane using diethylene glycol methyl ether as an internal standard. The performance characteristics of GC were evaluated in terms of selectivity, linearity, precision, accuracy, recovery, limit of detection (LOD) and limit of quantification (LOQ). The calibration curve was highly linear (the coefficient of determination: 0.9979) within the concentration range of $10.0{\sim}800.0{\mu}g/mL$ for MSM. The recoveries for three fortified concentrations were 96.7~97.1%, 96.6~97.3% and 96.8~97.2%, respectively. The LOD and LOQ of the method were $0.29{\mu}g/mL$ and $0.97{\mu}g/mL$, respectively. All obtained results were acceptable according to the guidelines of the Association of Official Analytical Chemists for dietary supplements. Thus, the validated analytical method using the GC-FID system is suitable for the determination of MSM in dietary supplement formulations for quality control.

• 한국환경보건학회지
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• 제32권1호
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• pp.67-70
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• 2006

A gas chromatography/mass spectrometric method was developed for the determination of formaldehyde in hair. 0.3mg of hair was placed in 10ml headspace vial. 1.5mM pentafluorophenylhydrazine solution (pH 2) in 0.03 M phosphoric acid and $20\;{\mu}l$ of 500 mg/l $acetone-d_6$ as internal standard were added in vial and sealed tightly with cap. The solution was heated for 30 min at $90^{\circ}C$ in heating block. The extraction, the derivatization and the evaporation were performed simultaneously. After heating of the solution, 0.5 ml of headspace was taken up and analyzed by gas chromatography-mass spectrometry (GC-MS). Low limit of detection (LaD) and Low limit of quantitation (LOQ) of formaldehyde were 0.5 and 1.5 ng/g, respectively. The method was used to analyze formaldehyde in rat hair after oral exposure. The developed method may be valuable to be used to analyze formaldehyde in human hair.

• Food Science and Biotechnology
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• 제18권4호
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• pp.895-899
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• 2009

A new approach for the determination of acrylamide (AM) in foods by solid phase microextraction-gas chromatography (SPME-GC) was established. AM was bromized and transformed to 2-bromoacrylamide (2-BAM). 2-BAM was then extracted by a commercial SPME fiber, $75-{\mu}m$ Car/PDMS fiber, for GC detection. The influence of extraction and desorption parameters such as extraction temperature and time, stirring rate, desorption temperature, and time were studied and optimized. The mass concentration was proportional to the peak area of 2-BPA from 1.0 to 8,000 ${\mu}g/L$. The detection limit of the SPME-GC for 2-BAM was found to be 0.1 ${\mu}g/L$, and the recoveries and relative standard deviations for different food samples were 74.5 to 102.0%, and 4.2 to 9.1%, respectively. The presented method was applied to the determination of AM in fried foods.