Hydrogen/Deuterium Exchange

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  • 8/13/2019 Hydrogen/Deuterium Exchange


    Research Topic task started on Thu Feb 5, 2004 at 2:36 PM

    2 Research Topic candidates were identified in CAPLUS.

    using the phrase "electrospray mass spectrometry"

    Selected 1 of 2 candidate topics.11692 references were found containing the concept "electrospray mass spectrometry".

    Research Topic Refine started

    150 references were found when refined using the phrase "deuterium exchange"


    CAPLUS: Copyright 2003 ACS (The UK patent material in this product/service is UK Crown copyright and is made

    available with permission. (C) Crown Copyright. The French (FR) patent

    material in this product/service is made available from Institut National de

    la Propriete Industrielle (INPI).)REGISTRY: Copyright 2003 ACS (Some records contain information from GenBank(R). See also: Benson D.A.,

    Karsch-Mizrachi I., Lipman D.J., Ostell J., Rapp B.A., Wheeler D.L.

    Genbank. Nucl. Acids Res. 28(1):15-18 (2000). Property values tagged

    with IC are from the ZIC/VINITI data file provided by InfoChem.)

    CASREACT: Copyright 2003 ACS (Some records from 1974 to 1991 are derived from the ZIC/VINITI data file

    provided by InfoChem. Some records are produced using some INPI data

    from the period prior to 1986.)

    CHEMLIST, CHEMCATS: Copyright 2003 ACS

    Bibliographic Information

    Dynamics and Ligand-Induced Solvent Accessibility Changes in Human Retinoid X Receptor Homodimer

    Determined by Hydrogen Deuterium Exchange and Mass Spectrometry. Yan, Xuguang; Broderick, David;

    Leid, Mark E.; Schimerlik, Michael I.; Deinzer, Max L. Departments of Chemistry, Biochemistry and Biophysics

    and Pharmaceutical Science, Oregon State University, Corvallis, OR, USA. Biochemistry (2004), 43(4), 909-

    917. CODEN: BICHAW ISSN: 0006-2960. Journal written in English. AN 2004:31167 CAPLUS (Copyright

    2004 ACS on SciFinder (R))


    Receptors for retinoic acid act as ligand activated transcription factors. The three-dimensional structure of the

    retinoid X receptor (RXR) ligand binding domain has been detd., but little information is available concerning the

    properties of the protein in soln. Hydrogen/deuterium exchange followed by electrospray ionization mass

    spectrometry was used to probe the soln. conformation of the recombinant human RXR homodimer ligand bindingdomain in the presence and absence of 9-cis-retinoic acid (9-cis-RA). Within the exptl. time domain (0.25-180 min),about 20 amide hydrogens showed decreased exchange rates in the presence of satg. concns. of 9-cis-RA as

    compared to those found for the homodimer in the absence of ligand. Most of the amides were located in peptides

    derived from regions of the protein shown by the X-ray structure to interact with the bound ligand: the amino

    termini of helixes 3 and 9, the two sheets, helix 8, the H8-H9 loop, and the carboxyl terminus of helix 11.Unexpectedly, protection was also obsd. in peptides derived from helixes 7, 10, 11, and the H7-H8 and H10-H11

    loops, regions that are not directly in contact with bound 9-cis-RA. These results suggest that the binding of ligand

    results in addnl. effects on the conformation or dynamics of the homodimer in soln. as compared to those obsd. for

    the X-ray structure. Overall, the change in deuterium exchange induced by the binding of 9-cis-RA correlated

  • 8/13/2019 Hydrogen/Deuterium Exchange


    reasonably well with changes in hydrogen bonding, residue depth, and/or solvent accessibility predicted from the

    crystal structure.

    Bibliographic Information

    Monitoring of high pressure protein denaturation by hydrogen/deuterium exchange and electrospray

    ionization mass spectrometry. Petry, Inga; Szewczuk, Zbigniew. Faculty of Chemistry, University of Wroclaw,Pol. Editor(s): Benedetti, Ettore; Pedone, Carlo. Peptides 2002, Proceedings of the European Peptide Symposium,

    27th, Sorrento, Italy, Aug. 31-Sept. 6, 2002 (2002), 854-855. Publisher: Edizioni Ziino, Castellammare di Stabia,

    Italy CODEN: 69EYXG Conference written in English. AN 2004:28713 CAPLUS (Copyright 2004 ACS on

    SciFinder (R))

    Bibliographic Information

    Elucidation of the fragmentation pathways of azaspiracids, using electrospray ionisation, hydrogen/deuterium

    exchange, and multiple-stage mass spectrometry. Sierra, Monica Diaz; Furey, Ambrose; Hamilton, Brett;

    Lehane, Mary; James, Kevin J. PROTEOBIO, Mass Spectrometry Centre for Proteomics and Biotoxin Research,

    Department of Chemistry, Cork Institute of Technology, Cork, Ire. Journal of Mass Spectrometry (2003),

    38(11), 1178-1186. CODEN: JMSPFJ ISSN: 1076-5174. Journal written in English. AN 2003:975783

    CAPLUS (Copyright 2004 ACS on SciFinder (R))


    Collision-induced dissocn. (CID) mass spectra were generated for azaspiracids using electrospray ionisation (ESI),

    and hydrogen/deuterium (H/D) exchange was used to ascertain the no. and type of replaceable hydrogens in the three

    predominant azaspiracid toxins. H/D exchange was conveniently achieved using deuterated solvents for liq.

    chromatog. (LC). Using ion-trap mass spectrometry, multiple-stage CID expts. (MSn) on the protonated and fully

    exchanged ions were performed to decipher characteristic fragmentation pathways. The precursor and product ions

    from azaspiracids lost up to five water mols. from different regions during MSn expts. and it was possible to

    distinguish between the water losses from different mol. regions. These studies confirmed that the first waterloss ion

    in the spectra of azaspiracids resulted from dehydration at the vicinal diol at C20-C21. Five MS dissocn. pathways

    were identified that resulted from fragmentation of the carbon skeleton of azaspiracids producing nitrogen-contg.

    ions. Two pathways, involving cleavage of the E-ring and C27-C28, gave ions that were found in all azaspiracids.Three pathways, A-ring, C-ring and C19-C20 cleavages, were useful for distinguishing between azaspiracid analogs.

    The same product ions from backbone fragmentation were also obsd. using hybrid quadrupole time-of-flight mass

    spectrometry (QqTOFMS). The fragmentation of the A-ring was the most facile and was exploited in the

    development of LC/MSn methods for the anal. of azaspiracids.

    Bibliographic Information

    Probing protein folding and binding by electrospray ionization Fourier transform mass spectrometry. Eyles,

    S. J.; Gumerov, D. R.; Gierasch, L. M.; Kaltashov, I. A. Departments of Chemistry, Polymer Science and

    Engineering, University of Massachusetts, Amherst, MA, USA. Advances in Mass Spectrometry (2001), 15

    499-500. CODEN: AMSPAH ISSN: 0568-000X. Journal written in English. AN 2003:974607 CAPLUS

    (Copyright 2004 ACS on SciFinder (R))


    The dynamics and ligand-binding mechanism of cellular retinoic acid binding protein I (CRABP I) were

    investigated. An amide H/D exchange was used to probe protein conformational stability. Mildly denaturing

    conditions were employed to increase the population of intermediate states. Structural anal. of folding intermediates

    was carried out by inducing dissocn. of protein ions in the gas phase and measuring the deuterium content of each

    fragment ion as a function of the H/D exchange time in soln. Preliminary data indicate that under mildly denaturing

    conditions, presence of RA leads to significant stabilization of the protein conformation.

  • 8/13/2019 Hydrogen/Deuterium Exchange


    Bibliographic Information

    Liquid chromatography-multiple tandem mass spectrometry for the determination of ten azaspiracids,

    including hydroxyl analogues in shellfish. Lehane, Mary; Saez, Maria Jose Fidalgo; Magdalena, Ana Brana;

    Canas, Isabel Ruppen; Sierra, Monica Diaz; Hamilton, Brett; Furey, Ambrose; James, Kevin J. Department of

    Chemistry, Mass Spectrometry Centre for Proteomics and Biotoxin Research, PROTEOBIO, Cork Institute ofTechnology, Cork, Ire. Journal of Chromatography, A (2004), 1024(1-2), 63-70. CODEN: JCRAEY ISSN:

    0021-9673. Journal written in English. AN 2003:967554 CAPLUS (Copyright 2004 ACS on SciFinder (R))


    Azaspiracids (AZAs) are a group of polyether toxins that cause food poisoning in humans. These toxins, produced

    by marine dinoflagellates, accumulate in filter-feeding shellfish, esp. mussels. Sensitive liq. chromatog.-electrospray

    ionisation mass spectrometry (LC-ESI-MSn) methods have been developed for the detn. of the major AZAs and their

    hydroxyl analogs. These methods, utilizing both chromatog. and mass resoln., were applied for the detn. of 10 AZAs

    in mussels (Mytilus edulis). An optimized isocratic reversed phase method (3 m Luna-2 C18 column) sepd. 10azaspiracids using acetonitrile/water (46:54, vol./vol.) contg. 0.05% trifluoroacetic acid (TFA) and 0.004%

    ammonium acetate in 55 min. Analyte detn. using MS3 involved trapping and fragmentation of the [M+H]+ and

    [M+H-H2O]+ ions with detection of the [M + H-2H2O]+ ion for each AZA. Linear calibrations were obtained forAZA1, using spiked shellfish exts., in the range 0.05-1.00 g/mL (r2 = 0.997) with a detection limit of 5 pg(signal:noise = 3). The major fragmentation pathways in hydroxylated azaspiracids were elucidated using

    hydrogen/deuterium (H/D) exchange expts. An LC-MS3 method was developed using unique parent ions and

    product ions, [M + H-H2O-C9H10O2R1R3]+, that involved fragmentation of the A-ring. This facilitated the

    discrimination between 10 azapiracids, AZA1-10. Thus, this rapid LC-MS3 method did not require complete

    chromatog. r