• Title/Summary/Keyword: Gas chromatography-mass spectrometry (GC/MS)

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Extraction and Bioassay of Allelochemicals in Jerusalem Artichoke

  • Sungwook Chae;Lee, Ho-Jin
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.46 no.4
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    • pp.309-316
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    • 2001
  • Helianthus tuberosus has been known to inhibit the growth of weeds and other plants sharing its habitat. This study was conducted to identify the allelochemicals of Helianthus tuberosus which were extracted with water and solvents. Aqueous extracts of leaf, stem, root, tuber and tuber peel of Helianthus tuberosus except tuber did not show significant differences in phytotoxicity to alfalfa seedlings. It was considered that Helianthus tuberosus contained fewer or less potential water-soluble substances that were toxic to alfalfa. Methanol extract of leaves of Helianthus tuberosus was sequentially partitioned in increasing polarity with n-hexane, ethylacetate and n-butanol. Each extract had a yield of 148, 12, 15.7 and 9.5g, respectively. Inhibitory effects on germination of alfalfa seeds treated with four fractions were not significantly different. But the significant reductions on hypocotyl length were observed for all the solvent extracts. Among the four fractions, the ethylacetate fraction showed the most significant inhibition effect on bioassay with alfalfa. Further separation of the active ethylacetate fraction by open column chromatography led to the 25 subfractions. In bioassay of each sub-fraction with alfalfa seeds, sub-fraction No. 13 showed the most inhibitory effect on seedling growth. $^1$H NMR and gas chromatography-mass spectrometry analysis revealed that sub-fraction No. 13 was the mixture of straight-chain saturated fatty acids.

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Structural Analyses of the Novel Phosphoglycolopids Containing the Unusual very Long Bifunctional Acyl Chain, α,ω-13,16-Dimethyloctacosanedioate in Thermoanaerobacter ethanolicus

  • Lee, Sang-Hoo;Kang, Se-Byung;Kim, Jai-Neung;Jung, Seun-Ho
    • Bulletin of the Korean Chemical Society
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    • v.23 no.12
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    • pp.1778-1784
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    • 2002
  • Novel membrane lipids containing the unusual very long chain fatty $acid{\alpha}{\omega}-1316-dimethyloctacosanedioate$, dimethyl. Ester (DME C30) was isolated and purified from thermophilic anaerobic eubacterium, Thermoanaerobacter ethanolicus. Structures of the lipids containing the bifunctional fatty acyl components were proposed by various analyses such as $^1H,\;^{13}C,\;^{31}P$ nuclear magnetic resonance (NMR), Fourier transform infrared(FTIR) spectroscopy, gas chromatography/mass spectrometry (GC/MS) and fast atom bombardment mass spectrometry (FAB/MS). Combined with the GC/MS, $^1H,\;and\;^{13}C$NMR data, we confirmed that the head groups of the lipids contained the glycerol and/or glucosamine molecules. $^{31}P$ NMR spectrum also showed that the lipids contained phosphate in a phosphodiester linkage. The proposed structures of these novel lipid components were the ones in which two head groups were linked by the membrane spanning fatty acyl component(DME C30)and regular chain fatty acids on glycerol moiety of each head group.

Simultaneous Determination of Urinary Phytoestrogens and Estrogens by Gas Chromatography/Mass spectrometry (GC/MS에 의한 뇨 중 Phytoestrogen과 Estrogen의 동시 분석)

  • Yang, Yoon Jung;Lee, Seon Hwa;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.374-385
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    • 1998
  • Phytoestrogens are biologically active compounds derived from plants foods. It had been suggested that phytoestrogens, by inhibiting aromatase in peripheral and/or cancer cells and lowering estrogen levels, may play a protective role as antipromotional compounds during growth of estrogen-dependent cancers. Therefore, simultaneous analysis of estrogens and phytoestrogens is necessary to elucidate the possible involvement of phytoestrogens in estrogen metabolism. In this view, we developed a simple and reproducible procedure to quantitatively determine estrogen and phytoestrogen metabolites. The proposed method consisted of solid phase extraction using preconditioned Serdolit AD-2 resin, enzyme hydrolysis with ${\beta}$-glucuronidase/arylsulfatase from Helix pomatia, liquid-liquid extraction and TMS-ether derivatization. And the final determination was carried out by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode (SIM). The precision and accuracy of this method was evaluated through within-a-day and day-to-day test. Recovery range and detection limit were 71.96~105.66%, 2~4 ng/mL, respectively. Using this method, 17 estrogen and 5 phytoestrogen compositions in urine of normal subjects were analyzed. It was found that amounts and relative distribution of urinary phytoestrigens and estrogens showed different pattern in male and female subjects.

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Analysis of Polycyclic Aromatic Hydrocarbons in Agricultural Soils by Gas Chromatography-Ion Trap Tandem Mass Spectrometry

  • Nam, Jae-Jak;Lee, Sang-Hak
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2003.11a
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    • pp.113-118
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    • 2003
  • An investigation has been carried out on collision-induced dissociation (CID) in the development of an analytical protocol for the determination of polycyclic aromatic hydrocarbons (PARs) by ion trap tandem mass spectrometry. Two different considerations were used to choose the optimal CID conditions for complex matrix environmental samples, namely, to determine the highest signal-to-noise (SIN) ratio and the other to eliminate the background interferences originated from complex matrix samples. The PAR content of agricultural soil was measured to estimate overall distribution of PAR in throughout the country, we collected and analyzed 226 soil samples from paddy and upland soil. The average content of total PAR in all samples was 236 ${\mu}g$ $kg^{-1}$, and the range was from 23.3 to 2, 834 ${\mu}g$ $kg^{-1}$. The overall distribution of PAR was found to be closely related to the pollution sources, the size of city and the type of industry.

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The Fate of Aspen Extractives in Kraft Pulping and Oxygen Delignification

  • Shin, Soo-Jeong;Lai, Yuan-Zong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.37 no.3
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    • pp.74-80
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    • 2005
  • The compositions of residual extractives in woodmeal, unbleached and oxygen-delignified aspen kraft pulps were investigated with gas chromatography(GC) and gas chromatography-mass spectrometry (GC-MS) with focus on fate of extractives in kraft pulping and oxygen delignification. Steryl esters and shorter retention time (shorter than palmitic acid) extractives were main extractives in aspen woodmeal. Shorter retention time extractives were well removed in kraft pulping. Sterol esters were hydrolyzed to sterols and fatty acids. Sterols and fatty acids were two major extractives classes in unbleached kraft pulps. Linoleic acid was main fatty acids in unbleached pulps compared with palmitic acid which is generally found in aspen woodmeal. Sterolsand fatty acids were also two major extractives classes in oxygen-delignified kraft pulps. However, linoleic acid was well removed in oxygen delignification.

Liquefaction Characteristics of Polypropylene-Polystyrene Mixture by Pyrolysis at Low Temperature (Polypropylene-Polystyrene 혼합물의 저온 열분해에 의한 액화특성)

  • Cho, Sung-Hyun;Kim, Chi-Hoi;Kim, Su-Ho;Lee, Bong-Hee
    • Clean Technology
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    • v.16 no.1
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    • pp.26-32
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    • 2010
  • The low temperature pyrolysis of polypropylene (PP), polystyrene (PS) and polypropylene-polystyrene (PP-PS) mixture in a batch reactor at the atmospheric pressure and $450^{\circ}C$ was conducted to investigate the synergy effect of PP-PS mixture on the yield of pyrolytic oil. The pyrolysis time was varied from 20 to 80 mins. The products formed during pyrolysis were classified into gas, gasoline, kerosene, gas oil and heavy oil according to the petroleum product quality standard of Ministry of Knowledge Economy. The analysis of the product oils by GC/MS(Gas chromatography/Mass spectrometry) showed that new components were not detected by mixing of PP and PS. There was no synergy effect according to the mixing of PP and PS. Conversions and yields of PP-PS mixtures were linearly dependent on the mixing ratio of samples except for heavy oil yields. Heavy oil yields showed almost constant regardless of the mixing ratio.

Determination of the presence of benzene in vitamin drinks using headspace - solid phase microextraction and gas chromatography - mass spectrometry (Headspace Solid Phase Microextraction-Gas Chromatography/Mass Spectrometry를 이용한 비타민드링크 제품 중 Benzene의 미량분석)

  • Kim, Jong-Hun;Lee, Kyung-Min
    • Analytical Science and Technology
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    • v.20 no.3
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    • pp.237-245
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    • 2007
  • The presence of benzene in 31 products of vitamin drinks purchased from 20 retail outlets was determined using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). The sample (25 ml) was stirred at 1200 rpm for 4 min using a magnetic bar with a $100{\mu}m$ SPME fiber as an adsorbent for benzene which was then desorbed from the fiber for 1 min in the GC injector. Quantitation was achieved using the standard addition method. The limit of detection was determined as 0.56 ng/ml and over a concentration range 0-40 ng/ml the coefficient of correlation was greater than 0.999. The concentration of benzene in the drinks examined was in the range not detectable to 47.35 ng/ml. Benzene was detected in 15 of the drinks with concentration in 5 of them greater than 10 ng/ml which is the limit set for the presence of benzene in the Drinking Water Regulations. The concentrations of benzene in the 5 drinks which exceeded the limit of 10 ng/ml were 16.99, 35.14, 16.03, 47.35 and 14.28 ng/ml respectively.

Analysis of Death Due to Poisoning in the National Capital Region (2014-2016) (수도권 부검시료에서 중독사 관련 사용물질 현황(2014-2016))

  • Park, Meejung;Park, Jongsin;Lee, Sangki;In, Sangwhan
    • Journal of The Korean Society of Clinical Toxicology
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    • v.15 no.2
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    • pp.101-106
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    • 2017
  • Purpose: This study examined the patterns of drugs, poisons, and chemicals detected in autopsy samples performed in the Seoul Institute and other regional forensic offices of the National Forensic Service (NFS) between 2014 and 2016. Methods: The investigation carried out using the laboratory information management system. Forensic toxicological identification and quantitation were performed in autopsy samples, including heart blood, peripheral blood, liver, kidney, vitreous humor and etc. Gas chromatography/mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) were used to analyze the drugs and poisons. Results: Forensic autopsies were performed on 9,674 cases in this period. Based on the autopsy reports, 699 cases (7.2%) were considered as unnatural deaths caused by fatal intoxication. The number of male deaths was higher than that of female deaths, with the age of 50-59 being the most common age group. Conclusion: Drugs comprised the largest number of deaths due to poison, followed by alcohol, agrochemicals, drug with alcohol, carbon monoxide, and cyanide, in that order. Zolpidem was the most frequently used drug in all drug-related intoxication cases.

Analysis of Agrochemical Residues in Tobacco Using Solid Phase Microextraction-Gas Chromatography with Different Mass Spectrometric Techniques

  • Lee, Jeong-Min;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Geon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.30 no.2
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    • pp.117-124
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    • 2008
  • A solid phase microextraction (SPME) method in combination with gas chromatography/mass spectrometric techniques was used for the extraction and quantification of 12 selected agrochemical residues in tobacco. The parameters such as the type of SPME fiber, adsorption/desorption time and the extraction temperature affecting the precision and accuracy of the SPME method were investigated and optimized. Among three types of fibers investigated, polyacrylate (PA), polydimethylsiloxane (PDMS) and polydimethylsiloxane-divinylbenzene (PDMS-DVB), PDMS fiber was selected for the extractions of the agrochemicals. The SPME device was automated and on-line coupled to a gas chromatograph with a mass spectrometer. Mass spectrometry (MS) was used and two different instruments, a quadrupole MS and triple quadrupole MS-MS mode, were compared. The performances of the two GC-MS instruments were comparable in terms of linearity (in the range of 0.01$\sim$0.5 $\mu$g/mL) and sensitivity (limits of detection were in the low ng/mL range). The triple quadrupole MS-MS instrument gave better precision than that of quadrupole MS system, but generally the relative standard deviations for replicates were acceptable for both instruments (< 15%). The LODs was fully satisfied the requirements of the CORESTA GRL. Recoveries of 12 selected agrochemicals in tobacco yielded more than 80% and reproducibility was found to be better than 10% RSD so that SPME procedure could be applied to the quantitative analysis of agrochemical residues in tobacco.

Volatile Component Analysis of Commercial Japanese Distilled Liquors (Shochu) by Headspace Solid-Phase Microextraction (헤드스페이스 고체상미량추출(Solid-Phase Microextraction)을 이용한 시판 일본소주의 휘발성 향기성분 분석)

  • Shin, Kwang-Jin;Lee, Seung-Joo
    • Korean Journal of Food Science and Technology
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    • v.47 no.5
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    • pp.567-573
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    • 2015
  • In this study, volatile compounds in nine commercial Japanese distilled liquors (Shochu) were isolated by headspace solid-phase microexrraction (SPME) and analyzed by gas chromatography (GC) and GC-mass spectrometry (MS). A total of 76 volatile components, including 48 esters, 13 alcohols, and 15 miscellaneous components, were identified. Esters and alcohols constituted the largest groups of quantified volatiles. Differences in volatile components among the distilled liquors and possible sample grouping were examined by applying principal component analyses to the GC-MS data sets. The first and second principal components explained 77.92% of the total variation across the samples. The samples using barley koji showed higher overall concentrations of total volatile components. Additionally, the principal component analysis did not reveal any sample grouping based on the raw material used.