• Title/Summary/Keyword: gas chromatography(GC)

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The Stimultaneous Determination of Phenolic Compounds by GC and GC/MS

  • Kim, Jong-Bae;Park, Jyung-Rewng
    • Preventive Nutrition and Food Science
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    • 제3권2호
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    • pp.111-118
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    • 1998
  • To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

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GC/MSD를 사용한 원유 내 잔류농약의 분석법 연구 (Research for the Analytical Method of Various Pesticides in Raw Milk by Gas Chromatography-Mass Spectrometry)

  • 오남수;신용국;백승천
    • 한국축산식품학회지
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    • 제29권4호
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    • pp.482-486
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    • 2009
  • The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

Determination of Acrylamide in Foods by Solid Phase Microextraction-Gas Chromatography

  • Chen, Liangbi;Liu, Haizhu;Yu, Ping;Zhao, Jinyun;Chen, Xi
    • 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.

Characterization of the Aroma of Salt-fermented Anchovy Sauce Using Solid Phase Microextraction-Gas Chromatography-Olfactometry Based on Sample Dilution Analysis

  • Kim, Hyung-Joo;Baek, Hyung-Hee
    • Food Science and Biotechnology
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    • 제14권2호
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    • pp.238-241
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    • 2005
  • Aroma-active compounds were evaluated from salt-fermented anchovy sauce by solid phase microextraction-gas chromatography-olfactometry (SPME-GC-O) based on sample dilution analysis (SDA). SPME extract from carboxen/polydimethylsiloxane (CAR/PDMS) fiber was the most similar to the original odor of salt-fermented anchovy sauce used for this experiment, followed by divinylbenzene/CAR/PDMS (DVB/CAR/PDMS) fiber. Because salt-fermented anchovy sauce contains 23% NaCl, NaCl concentration of diluent was considered when salt-fermented anchovy sauce was serially diluted. Linear relationship between GC response and sample concentration was observed when diluted with 23% NaCl solution, whereas not observed when diluted with deodorized distilled water. Eleven and 16 aroma-active compounds were detected by SPME-GC-O based on SDA using CAR/PDMS and DVB/CAR/PDMS fibers, respectively. Butanoic acid and 3-methyl butanoic acid showed the highest ${\log}_2SD$ factors for CAR/PDMS and DVB/CAR/PDMS fibers. Dimethyl trisulfide, methional, trimethyl amine, 1-penten-3-ol, and acetic acid were also detected as potent aroma-active compounds.

Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

  • Jung, Mi-Jin;Shin, Yeon-Jae;Oh, Se-Yeon;Kim, Nam-Sun;Kim, Kun;Lee, Dong-Sun
    • 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.

Transformation of dissolved organic matter in a constructed wetland: A molecular-level composition analysis using pyrolysis-gas chromatography mass spectrometry

  • Park, Jongkwan;Choi, Mijin;Cho, Jaeweon;Chon, Kyongmi
    • Environmental Engineering Research
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    • 제23권4호
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    • pp.390-396
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    • 2018
  • This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

Mass Spectrometer를 이용한 대두 배아 출추 Cerebroside의 구조 분석 (Structural Determination of Cerebrosides from Soybean Embryo by Mass Spectrometer)

  • 김정훈;장석윤;김여경
    • 분석과학
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    • 제6권3호
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    • pp.335-343
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    • 1993
  • Fast atom bombardment mass spectrometer(FAB-MS), gas chromatography mass spectrometer(GC-MS), TLC 등을 이용하여 대두 배아 추출 cerebroside의 구조를 분석하였다. Cerebroside를 이루고 있는 각각의 구성 성분은 화학적인 산분해 후 GC-MS로 분석하였다. Cerebroside의 분자량 분포는 LiOH로 포화된 3-nitrobenzyl alcohol(3-NBA)를 matrix로 한 양이온 검출 FAB-MS법으로 측정하였다. FAB-MS와 GC-MS 결과를 종합하여 cerebroside의 구조를 해석함으로써 기존의 분석법이 가지고 있던 문제점을 개선하였다. 대두 배아로부터 추출한 cerebroside의 대부분은 N-2'-hydroxy palmitoyl-sphingadienine에 당이 한 분자 결합된 형태로 존재하였으며 그 조성이 매우 단순하였다.

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생강(生薑)과 건강(乾薑)의 정유성분에 대한 GC 분석 실험 (Study on the Gas Chromatography of the Zingiberis Rhizoma and the Zingiberis Rhizoma Recens)

  • 최성모
    • 동의생리병리학회지
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    • 제22권5호
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    • pp.1236-1239
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    • 2008
  • The GC pictures were taken to investigate the difference between the Zingiberis Rhizoma and the Zingiberis Rhizoma Recens. For the Zingiberis Rhizoma Recens, there were many peaks in the GC pictures of the juice of that, but the decoction of that had vanished many big peaks and shown many new peaks. This result suggested that many elements had been created from the other elements. For the Zingiberis Rhizoma, even though it was similar to the decoction of the Zingiberis Rhizoma Recens, that had vanished many peaks. This result suggested that many elements had been vanished during the drying period.

두충엽의 휘발성 성분에 관한 연구 (Studies on the Volatile Compounds of Du-Chung Leaves)

  • 장희진;김옥찬
    • 한국식품과학회지
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    • 제22권3호
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    • pp.261-265
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    • 1990
  • 두충엽의 휘발성 성분을 SDE 장치로 추출한 후 GC 및 GC/MS에 의해서 비교 분석하였다. 확인된 성분은 35개 성분이며 alcohol류 7종, aldehyde류 3종, ketone류 4종, ester류 2종. hydrocarbon류 18종, phenol 1종이 확인되었다. 이 중에서 가장 많이 함유된 성분은 2-ethyl furyl acrolein으로 추정되었는데 전체 휘발성 성분의 31.4%를 차지하였다.

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