• 제목/요약/키워드: Mass Spectrometric

검색결과 259건 처리시간 0.022초

Application of a Gas Chromatography/Mass Spectrometric Method for the Determination of Butyltin Compounds in Sediment

  • Won, Yong-Il;Jung, Pyong-Gil;Chung, Min-Young;Kim, Byung-Joo;Yim, Yong-Heon;So, Hun-Young;Kim, Yong-Seong
    • Bulletin of the Korean Chemical Society
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    • 제25권10호
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    • pp.1508-1512
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    • 2004
  • A gas chromatography/mass spectrometric (GC/MS) method has been developed for the determination of trace mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT) compounds in sediments. Samples were extracted by 10% acetic acid in methanol containing 0.03% tropolone and were then derivatized for GC/MS analysis. Ethylation by sodium tetraethylborate and phenylation by sodium tetraphenylborate were evaluated as a derivatization reaction of the organotins in sample extract. n-Hexane was added into reaction media in the beginning of the reaction for the continuous extraction of derivatized organotins. Ethylation requires less than 2 hours to get proper derivatization yields for MBT, DBT, and TBT altogether and produces relatively low amounts of side reaction products. Compared to ethylation, phenylation requires much longer time but provides relatively lower yield and produces considerable amounts of side reaction products. Therefore, the ethylation reaction was applied for the analysis of organotin compounds in sediment. An isotope dilution mass spectrometric (IDMS) method based on GC/MS has been applied to the accurate determination of DBT compounds in the sediments. The IDMS results from the analyses of sediment samples showed a reasonable repeatability and a good agreement with the values obtained by IDMS based on liquid chromatography/induced coupled plasma/mass spectrometry.

Exploring the Mechanisms behind Disease using Mass Spectrometry

  • Byun, Jaeman
    • 한국독성학회:학술대회논문집
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    • 한국독성학회 2002년도 Current Trends in Toxicological Sciences
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    • pp.43-43
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    • 2002
  • Mass spectrometric study of oxidant damage: Generation of endogenous oxidizing species have been implicated in the pathogenesis of a wide variety of diseases from cancer to Alzheimer's Disease to Inflammatory bowel diseases. Antioxidant compounds may therefore be useful in treating or preventing these diseases.(omitted)

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Hydrolysis of Penicillin G and Carbenicillin in Pure Water - As Studied by HPLC/ESI-MS

  • Kolek, Marta;Franski, Rafal;Franska, Magdalena
    • Mass Spectrometry Letters
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    • 제10권4호
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    • pp.108-111
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    • 2019
  • The hydrolysis of penicillin G, carbenicillin and ampicillin in pure water at room temperature was studied by high pressure liquid chromatography electrospray ionization mass spectrometry. Hydrolysis of ampicillin did not occur under these conditions; however, penicillin G and carbenicillin were completely hydrolyzed after seven days. A short interpretation of this difference is proposed. The mass spectrometric behaviour, namely ESI response and fragmentation pathway, of hydrolyzed penicillin G and hydrolyzed carbenicillin have been also discussed.

Amino acid Thiohydantoin 유도체(誘導體)의 질량분석(質量分析) (제II보)(第II報) (Mass Spectrometric Identification of Thiohydantoins Derived from Amino Acids (II))

  • 송경덕
    • 한국식품영양과학회지
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    • 제3권1호
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    • pp.69-76
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    • 1974
  • The method of amino acid sequence determination from the C-terminal amino acid is proposed and mass spectrometric identification of thiohydantoins described previously. In this paper was discussed the fragmentation of thiohydantoin-ring by deutero substitution and model tripeptide have been degraded through three stages each, with interpretable results. The conditions employed in this method are mild enough for biological materials. The main features of the method are the following. 1. Thiohydantoins were formed in a non-aqueous medium a mixture of acetic anhydride, acetic acid and ammonium thiocyanate. 2. Mass sepectra of thiohydantoins derived from 20 amino acids were obtained with a mass spectrometer, JEOL model JMS-06H. 3. Cleavage of peptidyl thiohydantoin was made with an acidic from of a cation-exchange resin. (Amberlite IR-120) 4. Separation of the cleaved thiohydantoin and the parent peptide less one amino acid moiety was made by chromatography on a Sephadex G-10 column. 5. The peptide fraction was concentrated by freezedrying. 6. Thiohydantoin derivative of carboxyl terminal amino acid residue was introduced with a direct inlet probe in methanol solution.

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Determination of Methyl Bromide Used for the Preservation of Cultural Materials from Insects

  • Lee, Gil-Seung;Shin, Ueon-Sang;Shin, Ho-Sang
    • 한국환경보건학회지
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    • 제28권4호
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    • pp.27-30
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    • 2002
  • A thermal desorption-gas chromatography/mass spectrometric method was developed for the determination of methyl bromide in fumes formed during preservation of cultural materials from insects. Methyl bromide in lunes was collected by drawing 10ι of air through the adsorbent tube filled with a solid adsorbent (Chromosorb). The air samples were analyzed by using a special thermal desorption device and GC/MS determination. The recovery of methyl bromide by air sampling was 88% and the detection limit of the assay was 0.1 pptv based upon assayed air of 10ι. The method was applied to the determination of fumed methyl bromide used for the preservation of papers in a library. The mean concentration of methyl bromide determined in a library was 280.2 $\pm$ 25.4 pptv.

Liquid Chromatography-Tandem Mass Spectrometric Determination of Geniposide in Rat Plasma and its Pharmacokinetic Application

  • Jin, Ming Ji;Kim, In Sook;Kim, Dong-Hyun;Yoo, Hye Hyun
    • Bulletin of the Korean Chemical Society
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    • 제34권9호
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    • pp.2760-2764
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    • 2013
  • Geniposide is a biologically active ingredient of gardenia fruit. A liquid chromatography-tandem mass spectrometric method was developed and validated for the determination of geniposide in rat plasma. The plasma samples were pretreated by solid-phase extraction and introduced into a BDS Hypersil $C_{18}$ column ($50{\times}2.1mm$, $5{\mu}m$) for chromatographic separation. The mobile phase consisted of 0.1% formic acid and 0.1% formic acid in acetonitrile, and gradient elution was performed at a flow rate of 0.25 mL/min. For mass spectrometric detection, multiple reaction monitoring was performed via an electrospray ionization source in positive mode. The calibration curve for geniposide was linear ($r^2=0.997$) in the concentration range of $0.005-1{\mu}g/mL$. The intra- and inter-day accuracies and precisions fulfilled the required criteria (${\pm}15%$). The developed method was subsequently used for pharmacokinetic analysis of geniposide after oral administration to rats at a dose of 50 mg/kg. The mean maximum plasma concentration of geniposide was $0.68{\pm}0.29{\mu}g/mL$ at $0.44{\pm}0.13h$, and the mean area under the plasma concentration versus time curve was $1.46{\mu}g{\cdot}h/mL$.