• Title/Summary/Keyword: electrospray mass spectrometry

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A Study of in vitro Scavenging Reactions of Acrylamide with Glutathione Using Electrospray Ionization Tandem Mass Spectrometry

  • Cui, Sheng-Yun;Kim, Seung-Jin;Jo, Sung-Chan;Lee, Yong-Moon;Lee, Yong-Ill
    • Bulletin of the Korean Chemical Society
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    • v.26 no.8
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    • pp.1235-1240
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    • 2005
  • A combination of electrospray ionization and tandem mass spectrometry was used to characterize the scavenging reactions of acrylamide (AA) in the presence of glutathione (GSH) in vitro. In the presence of GSH, AA was deactivated effectively and scavenged by reactions consuming small amount of GSH. Reaction products and structural information were identified using collision-induced dissociation (CID) in an ion trap mass spectrometer. In the mixture of GSH and AA, significant increase in abundance of fragment ion peak was observed at m/z 233, which was identified as $[Cys-Glu]^+$, formed by the elimination of glycine moiety of GSH. GSH also contributes to the AA scavenging reaction by conjugating with AA through the sulfhydryl group in cysteine moiety. The probable scavenging reaction pathway of AA in the presence of GSH has been proposed based on the CID experimental data.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.

Mass Spectrometric Analysis for Discrimination of Diastereoisomers

  • Manshoor, Nurhuda;Weber, Jean-Fré
    • Mass Spectrometry Letters
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    • v.6 no.4
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    • pp.99-104
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    • 2015
  • A liquid chromatography mass spectrometry (LC-MS) system was used to identify and distinguish oligostilbene diastereoisomers. A polyphenolic extract from Neobalanocarpus heimii known to be rich in oligostilbenes of various degrees of condensation was used as test material. Fourteen oligostilbenes were isolated from this extract on a fully automated semi-preparative HPLC system. Out of these, two pairs of dimers, one pair of trimers, two pairs of tetramers and a group of four tetramers with similar skeleton were identified as diastereoisomers. Their structures and configurations were established by spectroscopic methods. All isolated compounds were subjected to an LC-MS/MS to study their fragmentation patterns. The experiments were performed on a liquid chromatography-mass spectrometry (LC-MS) with electrospray-ionization (ESI) interface in positive mode. MS/MS spectra of each pure compound were recorded by direct infusion in identical conditions and their product ion spectra were analysed. Some subtle yet significant differences were observed between the spectra of oligostilbenes from the various diastereoisomeric series.

Applications of Tandem Mass Spectrometry in the Structure Determination of Permethylated Sialic Acid-containing Oligosaccharides

  • Yoo, Eun-Sun;Yoon, In-Mo
    • Bulletin of the Korean Chemical Society
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    • v.26 no.9
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    • pp.1347-1353
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    • 2005
  • Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl($\alpha$ 2-3)Gal($\beta$ 1-3)GalNAc and sialyl($\alpha$ 2-3)Gal($\beta$ 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis.

Recent Progress on Microfluidic Electrophoresis Device Application in Mass Spectrometry

  • Roy, Swapan Kumar;Kim, Seongnyeon;Yoon, Jung H.;Yoon, Yong-Kyu;Cho, Kun
    • Mass Spectrometry Letters
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    • v.9 no.1
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    • pp.1-16
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    • 2018
  • Microfluidic technologies hold high promise and emerge as a potential molecular tool to facilitate the progress of fundamental and applied biomedical researches by enabling miniaturization and upgrading current biological research tools. In this review, we summarize the state of the art of existing microfluidic technologies and its' application for characterizing biophysical properties of individual cells. Microfluidic devices offer significant advantages and ability to handle in integrating sample processes, minimizing sample and reagent volumes, and increased analysis speed. Therefore, we first present the basic concepts and summarize several achievements in new coupling between microfluidic devices and mass spectrometers. Secondly, we discuss the recent applications of microfluidic chips in various biological research field including cellular and molecular level. Finally, we present the current challenge of microfluidic technologies and future perspective in this study field.

First Example of Monometallic Palladium(II) Compound with Trans-Chelating Tridentate Ligand: Synthesis, Crystal Structure, and Characterizations

  • Tae Hwan Noh
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.110-115
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    • 2023
  • The reaction of (COD)PdCl2 with new C3-symmetric tridentate L (COD = 1,5-cyclooctadien; L = 1,3,5-tris(picolinoyloxyethyl)cyanurate) in a mixture of acetone and dichloromethane produces single crystals consisting of unprecedented monometallacyclic [PdCl2(L)]. This cyclic compound arises from trans-chelation of two of three donating pyridyl groups of L, while the third pyridyl group remains uncoordinated. Electrospray ionization mass spectrometry (ESI-MS) data on L exhibited the major peak corresponding to [C27H24N6O9 + H+]+. Fast atom bombardment mass spectrometry (FABMS) data on [PdCl2(L)], however, showed the mass peak corresponding to the L instead of the present palladium(II) compound species, due to the insolubility and dissociation in solution. The physicochemical properties of the present palladium(II) compound were fully characterized by means of infrared (IR) and nuclear magnetic resonance (NMR) spectroscopy, thermal analysis, single-crystal X-ray diffraction (SC-XRD) measurement.

Solid Phase Extraction of Phospholipids from Brazil Nut (Bertholletia excelsa) and Their Characterization by Mass Spectrometry Analysis

  • Lima, Bruna R. De;Silva, Felipe M.A. Da;Koolen, Hector H.F.;Almeida, Richardson A. De;Souza, Afonso D.L. De
    • Mass Spectrometry Letters
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    • v.5 no.4
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    • pp.115-119
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    • 2014
  • The Brazil nut (Bertholletia excelsa - Lecythidaceae) is considered a product with high economic value, being a food widely appreciated for its nutritional qualities. Although previous studies have reported the biochemical composition of Brazil nut oil, the knowledge regarding the phospholipid composition exhibits a disagreement: the composition of fatty acids present in the structures of phospholipids is reported as being different from the composition of the free fatty acids present in the oil. In this work, solid phase extraction (SPE) was employed to provide a fast extraction of the phospholipids from Brazil nuts, in order to compare the phospholipid profile of the in nature nuts and their fatty acids precursor present in the oil. The major phospholipids were characterized by mass spectrometry approach. Their fragmentation pattern through direct infusion electrospray ionization ion-trap tandem mass spectrometry ($ESI-IT-MS^2$) proved to be useful to unequivocal characterization of these substances. High resolution (HR) experiments through ESI using a quadruple time of flight mass spectrometry (QTOF) system were performed to reinforce the identifications.

Fragmentation Analysis of rIAPP Monomer, Dimer, and [MrIAPP + MhIAPP]5+ Using Collision-Induced Dissociation with Electrospray Ionization Mass Spectrometry

  • Kim, Jeongmo;Kim, Ho-Tae
    • Mass Spectrometry Letters
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    • v.12 no.4
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    • pp.179-185
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    • 2021
  • Collision-induced dissociation (CID) combined with electrospray ionization mass spectrometry (ESI-MS) was used to obtain structural information on rat islet amyloid polypeptide (rIAPP) monomers (M) and dimers (D) observed in the multiply charged state in the MS spectrum. MS/MS analysis indicated that the rIAPP monomers adopt distinct structures depending on the molecular ion charge state. Peptide bond dissociation between L27 and P28 was observed in the MS/MS spectra of rIAPP monomers, regardless of the monomer molecular ion charge state. MS/MS analysis of the dimers indicated that D5+ comprised M2+ and M3+ subunits, and that the peptide bond dissociation process between the L27 and P28 residues of the monomer subunit was also maintained. The observation of (M+ b27)4+ and (M+ y10)3+ fragment ions were deduced to originate from the two different D5+ complex geometries, the N-terminal and C-terminal interaction geometries, respectively. The fragmentation pattern of the [MrIAPP + MhIAPP]5+ MS/MS spectrum showed that the interaction occurred between the two N-terminal regions of MrIAPP and MhIAPP in the heterogeneous dimer (hetero-dimer) D5+ structure.

Analysis of Amyloid Beta 1-16 (Aβ16) Monomer and Dimer Using Electrospray Ionization Mass Spectrometry with Collision-Induced Dissociation

  • Kim, Kyoung Min;Kim, Ho-Tae
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.177-183
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    • 2022
  • The monomer and dimer structures of the amyloid fragment Aβ(1-16) sequence formed in H2O were investigated using electrospray ionization mass spectrometry (MS) and tandem MS (MS/MS). Aβ16 monomers and dimers were indicated by signals representing multiple proton adduct forms, [monomer+zH]n+ (=Mz+, z = charge state) and [dimer+zH]z+ (=Dz+), in the MS spectrum. Fragment ions of monomers and dimers were observed using collision-induced dissociation MS/MS. Peptide bond dissociation was mostly observed in the D1-D7 and V11-K16 regions of the MS/MS spectra for the monomer (or dimer), regardless of the monomer (or dimer) charge state. Both covalent and non-covalent bond dissociation processes were indicated by the MS/MS results for the dimers. During the non-covalent bond dissociation process, the D3+ dimer complex was separated into two components: the M1+ and M2+ subunits. During the covalent bond dissociation of the D3+ dimer complex, the b and y fragment ions attached to the monomer, (M+b10-15)z+ and (M+y9-15)z+, were thought to originate from the dissociation of the M2+ monomer component of the (M1++M2+) complex. Two different D3+ complex geometries exist; two distinguished interaction geometries resulting from interactions between the M1+ monomer and two different regions of M2+ (the N-terminus and C-terminus) are proposed. Intricate fragmentation patterns were observed in the MS/MS spectrum of the D5+ complex. The complicated nature of the MS/MS spectrum is attributable to the coexistence of two D5+ configurations, (M1++M4+) and (M2+M3+), in the Aβ16 solution.

Study of Complexes of C2- and C6-dihydroceramides with Transition Metal Ions Using Electrospray Ionization Tandem Mass Spectrometry (ESI-MS/MS)

  • Lim, Jin-Yi;Kumar, Avvaru Praveen;Kim, Chang-Dae;Ahn, Chul-Jin;Yoo, Young-Jae;Lee, Yong-Ill
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.397-401
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    • 2009
  • The complexes of $C_2-\;and\;C_6$-dihydroceramides with transition metal ions have been investigated by using Electrospray ionization-tandem mass spectrometry (ESI-MS/MS). The formation and fragmentation pathways of several doubly charged cluster ions as well as singly charged cluster ions of $C_2-\;and\;C_6$-dihydroceramides with transition metal ions have studied by ESI-MS/MS in the positive mode. Under ESI conditions, dihydroceramides form singly and doubly charged complexes with transition metal ions $(Mn^{2+},\;Fe^{2+},\;Co^{2+},\;Ni^{2+},\;and\;Zn^{2+}\;except\;Cu^{2+})$ with the compositions of $[DHCer+M+2H^2O-H]^+,\;[2DHCer+M+2H2O-H]^+,\;[3DHCer+M+2H2O-H]^+,\;[2DHCer+M]^{2+},\;[3DHCer+M]^{2+},\;[4DHCer+M]^{2+},\;[5DHCer+M]^{2+},\;and\;[6DHCer+M]^{2+}\;(DHCer\;=\;C_2-\;or\;C_6$-dihydroceramide, M = transition metal ion). The different complexation behavior of copper is responsible for relatively lower affinity of dihydroceramides to copper compared to those of other transition metals. It is also found that in the mass spectrum of the dihydroceramide complexes with copper(II), [2DHCer+Cu-H]$^+$ was observed with considerable intensity as well as [2DHCer+Cu+2$H_2O-H]^+$ due to its different geometry from those of other metals.