• Title/Summary/Keyword: Electrospray ionization mass spectrometry

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Soft Ionization of Metallo-Mefenamic Using Electrospray Ionization Mass Spectrometry

  • Abdelhamid, Hani Nasser;Wu, Hui-Fen
    • Mass Spectrometry Letters
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    • v.6 no.2
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    • pp.43-47
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    • 2015
  • Detection of mefenamic acid (M, non-steroidal anti-inflammatory drug, NSAIDs) and its metallodrug was investigated using electrospray ionization mass spectrometry (ESI-MS) and fluorescence spectroscopy. ESI-MS data (500 µL, 1×10-3 M) revealed high detection sensitivity for the drug and metallodrug. ESI-MS spectra revealed peaks at 242, 580, and 777 Da corresponding to [M+H]+, [63Cu(M-H)2(H2O)2+H]+, and [56Fe(M-H)3+H]+, respectively. The metal:mefenamic ratios of ESIMS spectra are in complete agreement with the fluorescence spectroscopy results (1:2 for Cu(II) and 1:3 for Fe(III)). ESI is a soft ionization technique that can be used on labile metallo-mefenamic acids and is promising for the detection of these species in environmental samples and biological fluids.

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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    • v.10 no.4
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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.

General Fragmentations of Alkaloids in Electrospray Ionization Tandem Mass Spectrometry

  • Shim, Hee Jung;Lee, Ji Ye;Kim, Byungjoo;Hong, Jongki
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.79-82
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    • 2013
  • Various types of alkaloids observed in several herbal medicines were analyzed by electrospray ionization tandem mass spectrometry in positive ion mode. In the present study, MS/MS spectralpatterns were investigated for eight-types of alkaloids (aporpine, protoberberine, tetrahydroprotoberberine, benzylisoquinoline, protopine, phthalide, morpine, and bisbenzylisoquinoline). For aporpine- and protoberberine-type alkaloids, main fragmentations occurred at substituted groups on rigid ring structures, not showing ring fusion. Interesting fragmentations due to iminolization and retro-Diels-Alder (RDA) reaction were observed in MS/MS spectra of protopine- and tetrahydroprotobereberine-type alkaloids. Also, several types of fragmentations such as inductive cleavage and ${\alpha}$-cleavage, or bond cleavage between two ring structures were observed depending on their structural characteristics. These fragmentation patterns are expected to allow instant classification of the specific alkaloid type in various MS/MS spectra of alkaloids.

Determination of Enalapril in Human Plasma by High Performance Liquid Chromatography-Electrospray Ionization Mass Spectrometry

  • Yoon, Kyung-Hwan;Kim, Won;Park, Jong-Sei;Kim, Hie-Joon
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.878-880
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    • 2004
  • Revered-phase LC-electrospray ionization mass spectrometry was used to selectively determine enalapril from plasma with minimal sample preparation. Detection limit of the method was 1 ng/mL. Precision (within day and between days) and accuracy of the method at various concentrations were acceptable. The analytical technique was used for pharmacokinetic studies after administration of enalapril to human test subjects.

Mass spectrometry analysis system with integrated micro electrospray ionization emitter for peptide detection (펩타이드 질량 분석을 위한 전기 이온화 분사기의 제작 및 성능 평가)

  • Kim, Min-Su;Joo, Hwang-Soo;Kim, Byung-Gee;Kim, Yong-Kweon
    • Proceedings of the KIEE Conference
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    • 2007.07a
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    • pp.1534-1535
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    • 2007
  • This paper describes a novel microfluidic device with a microfabricated electrospray source for a sheathless electrospray ionization interface to a mass spectrometer. This electrospray ionization-mass spectrometry (ESI-MS) device consists of a triangular-shaped metal emitter, allowing the generation of an efficient electrospray for peptide detection, and microfluidic channels monolithically in a glass microchip. The performance of the proposed interface was evaluated by opimizing its experimental condition and spraying standard peptides. The spraying has high signal strength and stability, with a relative standard deviation of 2.9% and singly-charged and doubly-charged peaks of the peptides were successfully detected. The metal emitter source showed a good performance to be comparable to commercially available emitters in signal strength and stability.

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Identification of Ceftiofur Oxidation Products by High-Performance Liquid Chromatography/Electrospray Ionization/Tandem Mass Spectrometry

  • Lim, Young-Hee;Park, Deok-Hie;Youn, Yeu-Young;Kim, Kyung-Hoon;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • v.2 no.1
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    • pp.16-19
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    • 2011
  • Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

Application of Malononitrile Derivatization Method for Structural Glycomics Study in Matrix-assisted Laser Desorption/Ionization Time-of-flight Mass Spectrometry

  • Ahn, Yeong-Hee;Yoo, Jong-Shin
    • Journal of Photoscience
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    • v.8 no.2
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    • pp.83-86
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    • 2001
  • Structural analyses of oligosaccharide-malononitrile derivatives were conducted by matrix-assisted laser desorption/ionization post-source decay (MALDI-PSD) analysis in positive ion mode. The malononitrile derivatives of oligosaccharides, which were developed for highly sensitive detection of multi-component oligosaccharides by negative ion electrospray ionization mass spectrometry (ESI MS), were detected by positive-ion MALDI with the detection limit of 2 pmol level from the crude derivatization sample. The used matrix affected drastically the analytical results of oligosaccharide-malononitrile derivative by matrix-assisted laser desoprtion/ionization mass spectrometry (MALDI MS). The malononitrile derivatization of oligosaccharide also affect the patterns of MALDI-PSD spectra and give much more structural information than the free oligosaccharide.

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Examination of the Fragmentation Behavior of Hemin and Bilin Tetrapyrroles by Electrospray Ionization and Collision-induced Dissociation

  • Sekera, Emily R.;Wood, Troy D.
    • Mass Spectrometry Letters
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    • v.9 no.4
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    • pp.91-94
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    • 2018
  • Bilin tetrapyrroles are metabolic products of the breakdown of porphyrins within a species. In the case of mammals, these bilins are formed by the catabolism of heme and can be utilized as either biomarkers in disease or as an indicator of human waste contamination. Although a small subset of bilin tandem mass spectrometry reports exist, limited data is available in online databases for their fragmentation. The use of fragmentation data is important for metabolomics analyses to determine the identity of compounds detected within a sample. Therefore, in this study, the fragmentation of bilins generated by positive ion mode electrospray ionization is examined by collision-induced dissociation (CID) as a function of collision energy on an FT-ICR MS. The use of the FT-ICR MS allows for high mass accuracy measurements, and thus the formulas of resultant product ions can be ascertained. Based on our observations, fragmentation behavior for hemin, biliverdin and its dimethyl ester, phycocyanobilin, bilirubin, bilirubin conjugate, mesobilirubin, urobilin, and stercobilin are discussed in the context of the molecular structure and collision energy. This report provides insight into the identification of structures within this class of molecules for untargeted analyses.