• Title/Summary/Keyword: gas chromatography/mass spectrometry identification

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Identification of Homoserine Lactone Derivatives Using the Methionine Functionalized Solid Phase Synthesis by Gas Chromatography/Mass Spectrometry

  • Moon, Hong-Sik
    • Archives of Pharmacal Research
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    • v.27 no.1
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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.

Determination of panthenol, cholecalciferol and tocopherol in cosmetic products by gas chromatography-mass spectrometry in SIM mode

  • Hye-Jin Jeong;Myo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.22 no.2
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    • pp.153-160
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    • 1996
  • A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

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Identification of Volatile Flavor Components of Chinese chive and Baek-Seok Chie (중국 부추와 백석 부추의 휘발성 풍미 성분의 동정)

  • 이혜정;박희옥
    • The Korean Journal of Food And Nutrition
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    • v.10 no.4
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    • pp.539-543
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    • 1997
  • This study was carried out to investigate the Chinese and Baek-Seok chive. We collect the volatile components of Chinese and Baek-Seok chive by dynamic head space method. Chinese chive was analyzed by Gas chromatography-Mass Spectrometry(GC-MS). 28 components including 20 sulfides, 5 alcohols, 1 benzene and 2 aldehydes compounds were identified in samples, Also Baek-Seok chive was analyzed by GC-MS. 32 components including 19 sulfides, 10 alcohols, 2 benzonoides and 1 aldehyde compounds were confirmed.

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Analysis of 3,4-Methylendedioxymethamphetamine (MDMA) in Human Hair by Gas Chromatography/Mass Spectrometry (GC/MS를 이용한 모발 중 MDMA(Methylendedioxymethamphetamine)의 분석)

  • 박미정;김은미;임미애;정희선
    • YAKHAK HOEJI
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    • v.47 no.4
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    • pp.195-199
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    • 2003
  • An analysis method for the determination of methylendedioxymethamphetamine (MDMA) and its metabolite methylendedioxymethamphetamine (MDA) in hair by gas chromatography/mass spectrometry was proposed. For MDMA and MDA analysis, hair samples were incubated in MeOH (1% HCl), derivatized with trifluoroacetic anhydride and assayed by GC/MS. Hair of 18 subjects for drug abuse was analyzed for MDMA and MDA. Calibration curves for the determination of MDMA and MDA in hair showed a good linearity at a concentration range from 0.5 ng to 250 ng ($r^2$=0.999) The extraction recovery was determined from hair blanks at 50, 100 ng. The percentage of recovery were found to be 96.08∼103.48 with CV value of 1.62∼3.89. The concentrations of MDMA and MDA ranged 1.14∼38.06 ng/mg and 0.07∼3.91 ng/mg, respectively in 18 hair samples from MDMA abusers. The ratio of MDMA to MDA ranged from 9.65∼28.46 in all specimen. Hair analysis for MDMA is a useful method for identification of long-term drug abuser.

Extraction Methods of Organic Components from Rubber Composites and Analysis of the Extract Using Gas Chromatography/Mass Spectrometry

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.54 no.3
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    • pp.188-200
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    • 2019
  • Rubber articles contain various organic additives such as antidegradants, curing agents, and processing aids. It is important to extract and analyze these organic additives. In this paper, various extraction methods of organic additives present in rubber composites were introduced (solvent extraction, Soxhlet extraction, headspace extraction, and solid-phase microextraction), and the extracts were characterized using gas chromatography/mass spectrometry (GC/MS). Solvent and Soxhlet extractions are easy-to-perform and commonly used methods. Efficiency of solvent extraction varies according to the type of solvent used and the extraction conditions. Soxhlet extraction requires a large volume of solvent. Headspace sampling is suitable for extracting volatile organic compounds, while solid-phase extraction is suitable for extracting specific chemicals. GC/MS is generally used for characterizing the extract of a rubber composite because most components of the extract are volatile and have low molecular weights. Identification methods of chemical structures of the components separated by GC column were also introduced.

Flavor Components of the Needle Oils from Pinus rigida Mill and Pinus densiflora Sieb & Zucc (리기다송(Pinus rigida Mill)과 적송(Pinus densiflora Sieb & Zucc)잎 정유의 향기성분)

  • Choi, Kyoung-Sook;Park, Hyoung-Kook;Kim, Jung-Han;Kim, Yong-Taik;Kwon, Ik-Boo
    • Korean Journal of Food Science and Technology
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    • v.20 no.6
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    • pp.769-773
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    • 1988
  • The needle oils of Pious rigida Mill and Pious densiflora Sieb & Zucc were analyzed by gas chromatography/mass spectrometry. The major components of Pinus rigida were ${\alpha}-pinene$, 1-hexen-3-ol formate, sabinene, ${\beta}-pinene,\;{\alpha}-terpineol$ and ${\beta}-caryophyllene,\;{\alpha}-pinene$, bornyl acetate, ${\beta}-pinene$ and ${\beta}-hpellandrene$ were the major components fo Pious densiflora. Pious densiflora had sweeter and more greenish note than Pines rigida because the bornyl acetate content of Pious densiflora was about three times more than that of Pious rigida.

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Chiral Separation of Lactic Acid in Culture Media and Cells of Lactobacillus delbrueckii subsp. lactis as O-Pentafluoropropionylated (S)-(+)-3-Methyl-2-Butyl Ester by Achiral Gas Chromatography-Mass Spectrometry

  • Paik, Man-Jeong;Nguyen, Duc-Toan;Yoon, Jae-Hwan;Chae, Han-Seung;Kim, Kyoung-Rae;Lee, Gwang;Lee, Pyung-Cheon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.7
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    • pp.2418-2422
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    • 2011
  • The enantiomeric separation of lactic acid for its absolute configuration has become important task for understanding its biological origin and metabolic process involved in the formation of lactic acid. It involves the conversion of enantiomers as diastereomeric O-pentafluoropropionylated (S)-(+)-3-methyl-2-butyl ester and the direct separation by gas chromatography-mass spectrometry on a achiral capillary column. The (R)- and (S)-lactic acids were completely separated with a high resolution of 1.9. The newly developed method showed good linearity (r ${\geq}$ 0.999), precision (% relative standard deviation = 3.4-6.2), and accuracy (% relative error = -7.7-1.4) with the detection limit of 0.011 ${\mu}g/mL$. When the method was applied to determine the absolute configuration of lactic acid in Lactobacillus delbrueckii subsp. lactis 304 (LAB 304), the composition (%) of (R)-lactic acid in the cell pellet and in the culture medium were $89.0{\pm}0.1$ and $78.2{\pm}0.4$, respectively. Thus, it was verified that the present method is useful for the identification and composition test of lactic enantiomers in microorganisms.

Identification the Key Odorants in Different Parts of Hyla Rabbit Meat via Solid Phase Microextraction Using Gas Chromatography Mass Spectrometry

  • Xie, Yuejie;He, Zhifei;Lv, Jingzhi;Zhang, En;Li, Hongjun
    • Food Science of Animal Resources
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    • v.36 no.6
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    • pp.719-728
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    • 2016
  • The aim of this study was to explore the volatile compounds of hind leg, foreleg, abdomen and Longissimus dorsi in both male and female Hyla rabbit meat by solid phase microextraction tandem with gas chromatography mass spectrometry, and to seek out the key odorants via calculating the odor activity value and principal component analysis. Cluster analysis is used to study the flavor pattern differences in four edible parts. Sixty three volatile compounds were detected, including 23 aldehydes, 4 alcohols, 5 ketones, 11 esters, 5 aromatics, 8 acids and 7 hydrocarbons. Among them, 6 aldehydes and 3 acids were identified as the potential key odorants according to the ratio of concentration and threshold. The contents of volatile compounds in male Hyla rabbit meat were significantly higher than those in female one (p<0.05). The results of principal component analysis showed that the first two principal component cumulative variance contributions reach 87.69%; Hexanal, octanal, 2-nonenal, 2-decenal and decanal were regard as the key odorants of Hyla rabbit meat by combining odor activity value and principal component analysis. Therefore volatile compounds of rabbit meat can be effectively characterized. Cluster analysis indicated that volatile chemical compounds of Longissimus dorsi were significantly different from other three parts, which provide reliable information for rabbit processing industry and for possible future sale.

Pyrolysis/GC-Mass Spectrometry Analysis for Rapid Identification of Volatile Flavour Compounds of Accelerated Ripened Cheddar Cheese and Enzyme-Modified Cheese (단기숙성치즈 및 EMC 치즈의 휘발성 풍미성분 신속분석방법으로서 Pyrolysis/GC-Mass Spectrometry의 이용)

  • ;;;S.S.B. Haileselassie;V.A. Yaylayan;B.H. Lee
    • Food Science of Animal Resources
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    • v.21 no.3
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    • pp.256-264
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    • 2001
  • Pyrolysis/GC-mass spectrometry(Hewlet-Packard 5890GC/mass selective detector, 5971 BMSD), interfaced to a CDS Pyroprobe 1500 was optimized for rapid analysis of flavour compounds in Cheddar cheese. Twenty flavour compounds, including aldehydes(4), ketones(4), fatty acids(10), alcohol(1), and hydrocarbon(1), were identified from Cheddar cheeses. In total, Twenty-three flavour compounds aldehydes(2), ketones(8), alcohols(3), fatty acids(7), lactone(1), benzene derivative(1) and amide(1) were identified from two samples of accelerated-ripened Cheddar cheese treated with the proteolytic enzymes of Lactobacillus casei LGY. In total, Twenty-one flavour compounds; aldehydes(2), ketones(5), alcohols(2), fatty acids(11), and lactone(1) were identified from enzyme-modified cheese(EMC) treated with the combination of the proteolytic enzymes of Lactobacillus casei LGY and commercial endopeptidase or lipase. However, All the flavour compounds identified by pyrolysis/GC/MS in samples of ARC and EMC were not determined whether they are recognized as typical Cheddar flavour or not. More studies were requested on the development of methods for a rapid and convienent analysis of dairy fermented products using pyrolysis/GC-mass spectrometry.

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Separation and Identification of Polycyclic Aromatic Compounds in Pyrolysis Products of Cellulose and Lignin (셀룰로오스와 리그닌의 열분해 생성물중의 여러고리 방향족화합물의 분리와 동정)

  • Park, Nae-Joung;Lee, Milton L.
    • Journal of the Korean Chemical Society
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    • v.28 no.4
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    • pp.244-250
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    • 1984
  • Separation and identification of the polycyclic aromatic compounds (PAC) from pyrolysis products of cellulose and lignin were performed using a combination of acid-base solvent partitioning and silicic acid column chromatography with fused-silica capillary column gas chromatography/ mass spectrometry. Sixteen PAC were positively identifited by retention indices and mass spectra data. Both materials produced the same kinds of PAC. But lignin produced much more PAC than cellulose. Almost no highly carcinogenic heterocyclic PAC containing nitrogen and sulfur were produced.

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