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William Buchmann

Publications and source records attributed to William Buchmann.

7 recordsLinked to original sources

A study of noncovalent complexes involving single-stranded DNA and polybasic compounds using nanospray mass spectrometry.

Noncovalent complexes involving a single-stranded DNA oligonucleotide and a polybasic compound (spermine, penta-L-lysine, penta-L-arginine, or polydisperse poly-L-lysine) were detected by nanospray-MS. Several control experiments tended to show that these complexes preexisted in solution and that the interactions were initially ionic ones between oligonucleotide phosphates and protonated basic sites of the polybasic compound. Collision-induced dissociation (CID) experiments carried out with these complexes allowed us to identify some differences in the nature of the interactions between the solution and the gas phase, arising from possible proton transfers. Different dissociation pathways were observed according to the nature of the polybasic compound and to the initial charge state of the complex. The complex involving spermine dissociated by cleavage of noncovalent bonds leading to the separation of the two components, whereas the one involving penta-L-arginine underwent fragmentations of covalent bonds. Both behaviors were independent of the initial charge state of the complex. On the other hand, the dissociation pathway of the complex involving penta-L-lysine has been shown to be clearly charge state dependent. Noncovalent dissociation (separation of the two components) driven by coulomb repulsion occurred for the higher charged complexes, whereas fragmentation of covalent bonds was the main pathway of the lower charged complexes. In the latter case, differences in CID behavior were observed for different lengths of poly-L-lysine.

Biogenic Polyamines↗

Block lengths and block sequence of linear triblock and glycerol derivative diblock copolyethers by electrospray ionization--collision-induced dissociation mass spectrometry.

Chemical properties of ethylene oxide (EO) and propylene oxide (PO) block copolymers are strongly dependent on their sequence. Useful information about copolymer sequence can be obtained by tandem mass spectrometry (MS/MS). In this work, collision-induced dissociation (CID) of ammonium adducts of various linear triblock and glycerol derivative diblock copolyethers produced by electrospray ionization was studied under low-energy conditions. At first, homopolymers MS/MS spectra enabled us to identify the nature of the product ions and to suggest decomposition pathways. Then, it was shown that copolyethers with the same composition in each repeat unit but with inversed block sequences (i.e., PEO-b-PPO-b-PEO vs PPO-b-PEO-b-PPO and gPEO-b-PPO vs gPPO-b-PEO) can be easily distinguished with characteristic fragment ions. In the case of linear copolymers, CID spectra gave pertinent information about block lengths.

Epoxy Compounds↗

Analysis of poly(oxyethylene) and poly(oxypropylene) triblock copolymers by MALDI-TOF mass spectrometry.

Triblock copolymers of ethylene oxide (EO) and propylene oxide (PO) are widely used in the chemical industry as nonionic surfactants. Triblock copolymers can be arranged in a EO-PO-EO or PO-EO-PO sequence. This arrangement results in an amphiphilic copolymer, in which the block sequence and block length determine the properties of the copolymer. MALDI-TOF MS was used to analyze various triblock copolyethers: EO-PO-EO (Mn =2000 g.mol(-1)), PO-EO-PO (Mn = 2000 g.mol(-1)), and a random copolymer EO/PO (Mn = 2500 g.mol(-1)). Data treatment was assisted by using a homemade software allowing a picture of monomer composition of oligomers from the mass spectra. MALDI-TOF mass spectra of EO/PO copolymers were shown to depend strongly on the number of laser shots, relative proportions of polymer/salt, and the nature of the matrix. An unsaturated byproduct was detected. Its presence was demonstrated by prefractionation of copolymers by SEC before MALDI-TOF analysis, and its content was estimated by 1H NMR. The formation of layers inside the MALDI deposit was evidenced by varying the number of laser shots. Lighter oligomers of the copolymer, unsaturated byproduct, or both would be in the core of the deposit, coated with heavier oligomer. The layer formation depends on the nature of the matrix and the quantity of added salt. DHB matrix with a relative high sodium salt content induces layer formation inside the deposit, whereas dithranol matrix or low salt content does not. Consequently, an optimization of experimental parameters in order to estimate the lighter oligomers or unsaturated byproduct content or to obtain the actual representation of the monomer contribution in the copolymers from the MS data only seems obviously critical. MALDI-TOF mass spectrometry is obviously a powerful technique to analyze copolymers, but a careful survey of the experimental parameters is required. The combination of MALDI-TOF MS with separations techniques and NMR brings precious complementary information.

Anthralin↗

Characterization of peptides by liquid chromatography/electrospray ionization mass spectrometry using silver nitrate as a post-column complexant.

Two model peptides, des-Arg1-bradykinin (DAB) and bradykinin (B), were cationized by Ag+ after their separation by reversed-phase liquid chromatography (RPLC) prior to mass spectrometry (MS). Silver nitrate solution was used as a post-column reagent. The RPLC and MS experimental conditions were optimized using flow injection in order to obtain sufficiently abundant silver adducts to permit MS/MS experiments. The use of water-methanol with 0.1% formic acid as mobile phase allowed a good chromatographic separation of the two peptides with a polymeric stationary phase and sufficiently abundant silver-containing adducts, [M + Ag + H]2+ and [M + 2Ag]2+. The gas-phase dissociation of [DAB + Ag + H]2+ and [DAB + 2Ag]2+ led to interpretable mass spectra during the on-line cationization experiment. Most of the ions obtained by dissociating [DAB + Ag + H]2+ and [DAB + 2Ag]2+ species are silver-containing ions but the ions produced depend on the parent. The ions coming from the dissociation of the doubly charged silver adducts [DAB + Ag + H]2+ or [DAB + 2Ag]2+ are of interest compared with those coming from the singly charged silver species or doubly charged protonated species. The fragmentation of the doubly charged silver adducts provides ions over the entire mass range. Although the presence of several prolines in des-Arg1-bradykinin prevents the formation of some expected ions, the observation of triplets [an-H + Ag]+, [bn-H + Ag]+ and [bn + OH + Ag]+ produced by the dissociation of on-line Ag(+)-cationized peptides could contribute to greater success of automatic sequencing of peptides.

Bradykinin↗

Identification of water-soluble selenium-containing proteins in selenized yeast by size-exclusion-reversed-phase HPLC/ICPMS followed by MALDI-TOF and electrospray Q-TOF mass spectrometry.

An approach to speciation of selenium incorporated in yeast proteins was developed. The tryptic digest of a water-soluble protein fraction isolated by size-exclusion chromatography was analyzed by reversed-phase HPLC/ICPMS. The selenopeptides selected owing to the detector's elemental specificity were then analyzed by MALDI-TOFMS in order to select target ions for collision-induced dissociation MS. The latter, carried out with an electrospray Q-TOF spectrometer, enabled the sequencing of the selenopeptides detected by HPLC/ICPMS. The approach allowed for the first time the identification of a family of Se-containing proteins resulting from the replacement by selenomethionine of 2-9 methionine residues in a salt-stress-induced protein SIP18 (Mr 8874). The presence of these proteins was confirmed by MALDI-TOFMS of the original (nondigested) protein fraction. Another selenium protein identified was a heat-shock protein HSP12 (Mr 11693) in which the only methionine residue was replaced by selenomethionine. These two Se-containing proteins accounted for more than 95% of selenium in the water-soluble protein fraction.

Amino Acid Sequence↗

Detection of selenocompounds in a tryptic digest of yeast selenoprotein by MALDI time-of-flight MS prior to their structural analysis by electrospray ionization triple quadrupole MS.

MALDI-TOFMS was proposed as a key technique to a novel generic approach for the speciation analysis of selenium in yeast supplements. Owing to a lower detection limit and superior matrix tolerance to electrospray MS it allowed a successful detection of selenocompounds in samples for which electrospray MS had failed. The analytical approach developed was applied to the identification of a previously unreported selenopentapeptide (m/z 596) in the tryptic digest of a water-soluble selenoprotein fraction isolated by size-exclusion chromatography. The information on the mass of the protonated molecular ion obtained from MALDI allowed the optimization of the conditions for collision induced dissociation MS using a triple quadrupole spectrometer that enabled the determination of the amino acid sequence SeMet-Asn-Ala-Gly-Arg of the selenopeptide.

Dietary Supplements↗

Gas-phase ion/molecule reactions between dimethoxyphosphonium ions and aromatic hydrocarbons.

Ion/molecule reactions between O=P(OCH(3))(2)(+) phosphonium ions and six aromatic hydrocarbons (benzene, toluene, 1,2,4-trimethylbenzene, naphthalene, acenaphthylene and fluorene) were performed in a quadrupole ion trap mass spectrometer. The O=P(OCH(3))(2)(+) phosphonium ions, formed by electron impact from neutral trimethyl phosphite, were found to react with aromatic hydrocarbons (ArHs) to give (i) an adduct [ArH, O=P(OCH(3))(2)](+) and (ii) for ArHs which have an ionization energy below or equal to 8.14 eV, a radical cation ArH(+ *) by charge transfer reaction. Collision-induced dissociation experiments, which produce fragment ions other than the O=P(OCH(3))(2)(+) ions, indicate that the adduct ions are covalent species. Isotope-labeled ArHs were used to elucidate fragmentation mechanisms. The charge transfer reactions were investigated using density functional theory at the B3LYP/6-311 + G(3df,2p)//B3LYP/6-31G(d,p) level of theory. The potential energy surface obtained from B3LYP/6-31G(d,p) calculations for the reaction between O=P(OCH(3))(2)(+) and benzene is described.

Journal Article↗