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PubMed1994

Binding of 1,2(N)-dimethyl-6,7-dihydroxy-isoquinolinium ion to melanin: effects of ferrous and ferric ion on the binding.

1,2(N)-Dimethyl-6,7-dihydroxy-isoquinolinium ion (N-methylsalsolinium ion) was found to bind to melanin, while N-methyl(R)salsolinol and (R)salsolinol did not. Two components with different affinity to melanin were found; the dissociation constant and maximal binding capacity were obtained as 2.1 and 79.4 nM, and 103 and 1336 pmol/mg melanin, respectively. The binding was enhanced by ferrous ion markedly and inhibited by 1-methyl-4-phenylpyridinium ion and ferric ion. N-Methylsalsolinium ion may be accumulated in dopamine neurons as melanin conjugate, which is regulated by ferric and ferrous ions.

Ferric Compounds↗
PubMed1993

Non-invasive sampling of lactic acid ions by iontophoresis using chloride ion in the body as an internal standard.

Non-invasive sampling of lactic acid, as a model endogenous compound, through hairless rat skin by iontophoresis was investigated using a two-chamber iontophoretic diffusion cell equipped with platinum electrodes and a pulse depolarization iontophoretic system. Chloride ion in the body was used as an internal standard. First, an in vitro experiment on the permeation of lactate and chloride ions through hairless rat skin was carried out to determine the flux ratio of these ions. The cathode side of the cell (dermis side) was filled with physiological saline containing lactic acid (0.5556, 1.111, 1.667 or 2.222 mmol cm-3) and the anode side (epidermis side) with phosphate buffer (pH 7.4). The amount of lactate and chloride ion permeated from the dermis side to the epidermis side through the skin at a constant current of 3.0 mA was determined using an automatic lactic acid analyser and high-performance ion chromatography, respectively. For construction of a calibration curve of lactic acid in the dermis side, the ionic mobility ratio of lactic acid/chloride ion (UCl/Ulac) was determined using a computer simulation program from the flux ratio of lactic acid and chloride ion and the applied concentration of lactic acid in the dermis side. Second, an in vitro non-invasive sampling experiment of lactic acid through rat skin was carried out at a constant current of 2.0 or 3.0 mA and 2.222 or 1.111 mmol cm-3 of lactic acid in the dermis side, respectively.(ABSTRACT TRUNCATED AT 250 WORDS)

Animals↗
PubMed2005

Interactions between metal ions and carbohydrates. The coordination behavior of neutral erythritol to lanthanum and erbium ions.

Lanthanide ions and erythritol form metal-alditol complexes with various structures. Lanthanum nitrate and erbium chloride coordinate to erythritol to give new coordination structures. The lanthanum nitrate-erythritol complex (LaEN), 2La(NO3)3.C4H10O(4).8H2O, La3+ exhibits the coordination number of 11 (namely 11 polar atoms bound to one lanthanum) and is 11-coordinated to two hydroxyl groups from one erythritol molecule, six oxygen atoms from three nitrate ions and three water molecules. One erythritol molecule is coordinated to two La3+ ions and links the two metal ions together. The ratio of M:L is 2:1. The erbium chloride-erythritol complex (ErE), ErCl2.C4H9O(4).2C2H5OH was obtained from ErCl3 and erythritol in aqueous ethanol solution and the structure shows that deprotonation reaction occurs in the reaction process. The Er3+ cation is 8-coordinated with three hydroxyl groups of one erythritol molecule, two hydroxyl groups from another erythritol molecule, two ethanol molecules, and one chloride ion. Erythritol provides its three hydroxyl groups to one erbium cation and two hydroxyl groups to another erbium cation, that is, one hydroxyl group is coordinated to two metal ions and therefore loses its hydrogen atom and becomes a oxygen bridge. Another chloride ion is hydrogen bonded in the structure. The results indicate the complexity of metal-sugar coordination.

Crystallization↗
PubMed2005

High amplitude short time excitation: a method to form and detect low mass product ions in a quadrupole ion trap mass spectrometer.

Collision induced dissociation (CID) in a quadrupole ion trap mass spectrometer using the conventional 30 ms activation time is compared with high amplitude short time excitation (HASTE) CID using 2 ms and 1 ms activation times. As a result of the shorter activation times, dissociation of the parent ions using the HASTE CID technique requires resonance excitation voltages greater than conventional CID. After activation, the rf trapping voltage is lowered to allow product ions below the low mass cut-off to be trapped. The HASTE CID spectra are notably different from those obtained using conventional CID and can include product ions below the low mass cut-off for the parent ions of interest. The MS/MS efficiencies of HASTE CID are not significantly different when compared with the conventional 30 ms CID. Similar results were obtained with a two-dimensional (linear) ion trap and a three-dimensional ion trap.

Journal Article↗
PubMed2006

Characterization of cardiolipin from Escherichia coli by electrospray ionization with multiple stage quadrupole ion-trap mass spectrometric analysis of [M - 2H + Na]- ions.

We report a multiple-stage ion-trap (IT) mass spectrometric approach with electrospray ionization (ESI) for structural characterization of the [M - 2H + Na]- ion of cardiolipin (CL), a 1,3-bisphosphatidyl-sn-glycerol that consists of four fatty acyl chains and three glycerol backbones designated as A, B, and central glycerol, respectively (see Scheme 1). Following collisionally activated dissociation (CAD), the [M - 2H + Na]- ions of CL yield two prominent fragment ions that arise from the differential losses of the diacylglycerol moieties containing A or B glycerol, respectively. The tentative assignment of the two phosphatidyl moieties attached to the 1'- or 3'-position of the central glycerol is based on the observation that the ions arising from loss of the diacylglycerol moiety containing glycerol B is more abundant than that containing glycerol A. The structures of the above two ions, including the identities of the fatty acyl substituents and the position of fatty acyl substituents on the glycerol backbones (glycerol A and B) are determined by MS3 experiments that give spectra comprising several sets of prominent ions informative for the structural assignment of the fatty acyl substituents on the glycerol A and glycerol B. This method permits the structures of CL in a mixture isolated from Escherichia coli, including species that consist of various isomers, to be unveiled in detail.

Cardiolipins↗
PubMed2005

Fluorescence study of the interaction of Suwannee River fulvic acid with metal ions and Al3+-metal ion competition.

In this study emission and synchronous-scan fluorescence spectroscopy have been used to investigate the interaction of the class A (oxygen seeking 'hard acid') metal Al(3+), with Suwannee River fulvic acid (SRFA), as well as competition between Al(3+) and several other metal ions (Ca(2+), Mg(2+), Cu(2+), Pd(2+), La(3+), Tb(3+) and Fe(3+)) for binding sites on SRFA. Of the four metal ions possessing very similar (and relatively low) ionic indices (Ca(2+), Mg(2+), Cu(2+) and Pd(2+)) only the latter two paramagnetic ions significantly quenched SRFA fluorescence emission intensity. Of the four metal ions possessing very similar (and relatively low) covalent indices (Ca(2+), Mg(2+), La(3+) and Tb(3+)) only the last paramagnetic ion (Tb(3+)) significantly quenched SRFA fluorescence. None of these metals was able to significantly compete with SRFA-bound Al(3+).Fe(3+), which differs substantially from all of the other metals examined in this study in that it possesses a relatively high ionic index (but not as high as Al(3+)) and a relatively low covalent index (but not as low as Al(3+)), was able not only to quench SRFA fluorescence but also to compete (at least to some extent) with SRFA-bound Al(3+). Synchronous-scan fluorescence SRFA spectra taken in the absence and presence of Fe(3+) and/or Al(3+) support the view that these two metal ions can compete for sites on SRFA. The results of these fluorescence experiments further confirm the Al(3+), and metal ions that have electronic properties somewhat similar to Al(3+) (such as Fe(3+)) are somewhat unique in their ability to interact strongly with binding sites on fulvic acids.

Journal Article↗
PubMed2004

Comparison of the ion exchange uptake of ammonium ion onto New Zealand clinoptilolite and mordenite.

In this study the uptake performances of the naturally occurring zeolite, clinoptilolite, and of New Zealand mordenite are compared. The uptake of fully ionised ammonium ion from aqueous solutions in the concentration range 0-200 mg/l on to these two materials was compared. The influence of other cations present in water upon the ammonia uptake was also determined. The cations studied were potassium, calcium and magnesium. In all cases the anionic counterion present was chloride. The results showed that the mordenite exhibited higher overall uptake concentrations at equilibrium compared with clinoptilolite at solution concentrations greater than 80 mg/l. Beyond this value, the difference in solid-phase equilibrium concentrations on the mordenite became greater at higher solution-phase ammonium ion concentrations. The effect of the other cations upon uptake of ammonium ion was relatively small. In all cases, the ammonium ion showed the highest uptake on to both the mordenite and the clinoptilolite. In the case of clinoptilolite this was rather an unexpected result since the majority of other work shows clinoptilolite exhibiting a higher affinity for potassium ion compared with ammonium ion. This may be explained by the fact that the clinoptilolite came from volcanic deposits in New Zealand. This is the first such study on this material. At solution-phase equilibrium concentrations of greater than 80 mg/l, the mordenite showed smaller reductions in ammonium ion uptake in the presence of the other cations when compared with clinoptilolite.

Aluminum Silicates↗
PubMed1972

Current-voltage curves of porous membranes in the presence of pore-blocking ions. I. Narrow pores containing no more than one moving ion.

We propose a physical model for voltage-dependent conductance changes of excitable cell membranes. It is based on competition of uni- and bivalent ions for chains of stable sites extending through the membrane. These one-dimensional pathways (pores) have different profiles of chemical potential for the two ionic species so that bivalent ions can block the passage of univalent ions at large membrane potentials. We treat the special case that each pore is either empty or, because of electrostatic repulsion, contains no more than one uni- or bivalent ion at a time. A system of linear differential equations describes the time-dependent probabilities of the various possible pore states. The states are limited by transition rate constants involving the profile of the chemical potential, the membrane voltage, the ionic concentrations in the adjacent baths, and electrostatic interactions between the ions. The steady-state solutions (Kirchhoff-Hill theorem) yield expressions for the relationship between the small signal conductance of univalent ions and the concentration of these ions in the external bathing medium (a saturation curve) and for the ionic currents and the steady-state current-voltage curve (N-shaped). From the latter curve we compute the shift of theshold potential caused by concentration changes of the external bathing medium. The model yields a number of predictions which can be tested experimentally.

Binding Sites↗
PubMed1997

Ion chromatographic characterization of toxic solutions: analysis and ion chemistry of biological liquids.

The literature on the analysis of biological fluids by ion chromatography is reviewed herein. It has been demonstrated that ion chromatography is the method of choice for the determination of anions such as chloride, nitrite, bromide, phosphate, nitrate, sulfate, oxalate, thiocyanate, thiosulfate, citrate, isocitrate, carbonate, and similar species. Cations such as sodium, ammonium, potassium, magnesium, and calcium in various biological solutions have also been successfully identified and quantified. The technique fulfils several requirements of a reliable microanalytical method by providing sufficient speed, automation, case of use, and accuracy. For many types of analyses, very little or even no sample preparation is required. Because of this, as presented in this review, ion chromatography is widely used not only to obtain reliable clinical data, but also to study ion chemistry. It has been an invaluable tool in nephrolithiasis and dental research. This review should provide a useful reference for analysts and researchers involved in clinical studies. The review is presented in four sections: (1) introduction, (2) methods of analysis, (3) ion chemistry and (4) critical comments and concluding remarks. Section 1, as usual, deals with the general introduction of the subject and objectives. Section 2 includes the review of the literature on ion chromatography (IC) methods developed for routine analysis of various analytes present in biological fluids. Section 3 deals with the applications of IC used in the understanding of ion chemistry of biological fluids. Specifically, it deals with the physical chemistry aspects related to nephrolithiasis and dental research, such as speciation, driving force for crystals formation and crystallization, and pathophysiology. Section 4 contains critical comments and concluding remarks.

Animals↗
PubMed1982

Reversed-phase ion-pair high-performance liquid chromatographic assay of 5-fluorouracil, 5'-deoxy-5-fluorouridine, their nucleosides, mono-, di-, and triphosphate nucleotides with a mixture of quaternary ammonium ions.

Several quaternary ammonium ions were evaluated in the development of a reversed-phase ion-pair high-performance liquid chromatographic assay for the separation of the known nucleosides and nucleotides of 5-fluorouracil (FU) and its analogue, 5'-deoxy-5-fluorouridine (5'-dFUR). The capacity factors of FU, 5'-dRUR, and their eight anabolites including 5-5-fluorouridjine and its mono-, di-, triphosphate and diphosphoglucose, 5-fluorodeoxyuridine and its mono;- and diphosphate nucleotides, were dependent on the chain length and concentration of the counter ions, pH, type of buffer, as well as the type of bonded stationary phase. Separation of FU, 5'-dFUR, their nucleosides and monophosphate nucleotides was readily achieved using tetrabutylammonium ion alone as the counter ion. However, under these conditions, the di- and triphosphate nucleotides were eluted from the column only after lengthy gradient elution and with poor reproducibility. Optimal conditions for a simultaneous separation of the ten fore-mentioned compounds were achieved using a two-step elution with a mixture of tetraethylammonium (C8) and tetrabutylammonium (C16) ions. The first eluent consisted of C8 and C16 ions in a mixture of acetate--phosphate buffer and methanol, the second eluent contained an additional 30 mM phosphate. FU, 5'-dFUR, their nucleosides and monophosphates and diphosphoglucose were separated by isocratic elution from a microBondapak C18 reversed-phase column using the first eluent; and the di- and triphosphate nucleotides were subsequently eluted, isocratically with the second eluent. This assay does not require gradient elution and can be completed within 50 min with good reproducibility.

Chromatography, High Pressure Liquid↗
PubMed2002

Poly(ethylene glycol) doubly and singly cationized by different alkali metal ions: relative cation affinities and cation-dependent resolution in a quadrupole ion trap mass spectrometer.

Structural information of gas phase complexes of poly(ethylene glycol) (PEG) cationized by one or two different alkali metal ions is inferred from MS and MS/MS experiments performed with an electrospray quadrupole ion trap mass spectrometer. The rationale for selecting PEG was that its sites for cation binding are non-selective with respect to the repeating monomeric unit of the polymer, but there is selectivity with respect to the formation of an inner coordination sphere specific to each metal ion. The dissociation of [M1+ M2+ (EO23)], where EO23 = linear polymer of ethylene oxide, 23 units in length, resulted in loss of one of the alkali metal ions, with preference for loss of the larger cation, with no fragmentation of the PEG backbone for Na, K, Rb, and Cs. Li was not examined in this portion of the study. The selectivity for loss of the larger alkali metal ion was [Na+ K+ (EO23)] to [Na+ (EO23)] + K+ at 100%; [K+ Rb+ (EO23)] to [K+ (EO23)] + Rb+ at 93%; and [Rb+ Cs+ (EO23)] to [Rb+ (Eo23)] + Cs+ at 99%. The resolution of [M+ (EOx)] for x = 20-30 was dependent on the alkali metal ion, with the highest resolution observed for Cs+ and the lowest for Na+. These results are discussed with respect to the packing of the oxygen atoms on PEG (M.W.(avg) = 1000) around an alkali metal ion of different radius, and how this packing leads to an ensemble of unique structures, and therefore mobilities for [M+ (EOx)].

Journal Article↗
PubMed2002

Branching pattern and sequence analysis of underivatized oligosaccharides by combined MS/MS of singly and doubly charged molecular ions in negative-ion electrospray mass spectrometry.

We previously reported that sequence and partial linkage information, including chain and blood-group types, of reducing oligosaccharides can be obtained from negative-ion electrospray CID MS/MS on a quadrupole-orthogonal time-of-flight instrument with high sensitivity and without derivatization (Chai, W.; Piskarev, V.; Lawson, A. M. Anal. Chem. 2001, 73, 651-657). In contrast to oligonucleotides and peptides, oligosaccharides can form branched structures that result in a greater degree of structural complexity. In the present work we apply negative-ion electrospray CID MS/MS to core-branching pattern analysis using nine 3,6-branched and variously fucosylated oligosaccharides based on hexasaccharide backbones LNH/LNnH as examples. The important features of the method are the combined use of CID MS/MS of singly and doubly charged molecular ions of underivatized oligosaccharides to deduce the branching pattern and to assign the structural details of each of the 3- and 6-branches. These spectra give complimentary structural information. In the spectra of [M - H]-, fragment ions from the 6-linked branch are dominant and those from the 3-linked branch are absent, while fragment ions from both branches occur in the spectra of [M - 2H]2-. This allows the distinction of fragment ions derived from either the 3- or 6-branches. In addition, a unique D2beta-3 ion, arising from double D-type cleavage at the 3-linked glycosidic bond of the branched Gal core residue, provides direct evidence of the branching pattern with sequence and partial linkage information being derived from C- and A-type fragmentations, respectively.

Adult↗
PubMed2002

On the importance of ions and ion-molecule reactions to plasma-surface interface reactions.

Ions are known to be key players in many plasma processes, including anisotropic etching, film deposition and surface modification. The relationship between plasma ions, film properties, and surface interactions of other plasma species is not, however, well known. Using our Imaging of Radicals Interacting with Surfaces (IRIS) technique, along with plasma ion mass spectrometry (PI-MS), and surface analysis data, we have measured the effects of ion bombardment on the surface interactions of SiF2 in SiF4 plasmas and of CF2 in C3F8 and C4F8 plasmas. SiF2 is a known product of F-atom etching of Si, and CF2 has also been cited as a product of fluorocarbon etching of Si. With both molecules, we measure surface generation when the surface is bombarded by all the plasma species. Removal of ions from the plasma molecular beam results in a net decrease in surface generation for both molecules at all powers. Results in both systems are compared with the gas-phase ion-molecule reaction data of Armentrout and coworkers. Preliminary guided-ion beam mass spectrometry results taken in the Armentrout laboratories for the Ar+ + C3F8 reaction system are also presented.

Journal Article↗
PubMed2003

Ammonium ion mediated resorcarene capsules: ESI-FTICRMS study on gas-phase structure and ammonium ion affinity of tetraethyl resorcarene and its per-methylated derivative.

The ammonium ion binding affinities of tetraethyl resorcarene (1) and its per-methylated derivative (2) were studied by electrospray ionization Fourier transform ion cyclotron resonance (ESI-FTICR) mass spectrometry. Ten different ammonium ions were tested as guests for the resorcarenes. A strong tendency for complex formation was observed with all ammonium ions of size and charge distribution suitable for noncovalent interactions with the cavities of the resorcarene hosts 1 and 2. Although differences in ammonium ion affinities were observed between 1 and 2 due to the dissimilar conformations, the overall tendency was that increase in the degree of substitution and the length of carbon chain of the ammonium cation facilitated the complex formation until the sterical hindrance impeded the complexation. Dimeric as well as monomeric ammonium ion complexes were formed with resorcarene 1, but resorcarene 2 was unable to form the dimeric capsules because of the lack of H-bond donor possibilities. The nature of binding of the guest was further investigated with ion-molecule reactions and by determination of the single crystal X-ray structure of host 1 complexed with tetramethyl ammonium bromide.

Journal Article↗
PubMed1993

Structurally diagnostic ion-molecule reactions and collisionally activated dissociation of 1,4-benzodiazepines in a quadrupole ion trap mass spectrometer.

The ion-molecule reactions of various 1,4-benzodiazepines and dimethyl ether ions were studied with a quadrupole ion trap mass spectrometer. The methoxymethylene ions of dimethyl ether selectively react with 3-hydroxy-1,4-benzodiazepines (temazepam, oxazepam) to form (M+13)+ adducts by methylene substitution, and they react with 1,4-benzodiazepines that do not have hydroxyl substituents (diazepam, nordiazepam, nitrazepam) to form (M+15)+ adduct by a simple methyl cation transfer. These adducts are formed by elimination of methanol or formaldehyde, respectively, from (M+CH2OCH3)+ precursor ions. Ion-molecule reactions of model compounds with dimethyl ether ions suggest that the reactive site in the formation of (M+15)+ adducts is the imine functional group of the 1,4-benzodiazepines, while the reactive site for formation of (M+13)+ adducts involves a functional group interaction between the hydroxyl and carbonyl functional groups. Fragmentation induced by chemical ionization and collisionally activated dissociation provides further structural information for the differentiation of 1,4-benzodiazepines. Also, the gas-phase basicities of diazepam and temazepam have been estimated by bracketing techniques to be between 220.7 and 222.2 kcal/mol.

Benzodiazepines↗
PubMed1993

Automatic precursor-ion switching in a four-sector tandem mass spectrometer and its application to acquisition of the MS/MS product ions derived from a partially (18)O-labeled peptide for their facile assignments.

We developed an acquisition processor unit to control MS1 and MS2 in a four-sector tandem mass spectrometer simultaneously. The magnetic field strength of MS1 corresponding to the precise centers of the precursor ions, whose masses are determined by MS1 in advance, is recalibrated using an appropriate standard just before an MS/MS experiment, which allows consecutive acquisition of the MS/MS spectra from multiprecursor ions by B2/E2-linked scanning of MS2 synchronized with automatic B1 switching to the centers of each precursor ion on MS1. The accuracy of the automatic precursor-ion switching and the efficiency of consecutive B2/E2-linked scannings were demonstrated by measurement of a peptide mixture. The new MS/MS control system was further applied to rapid acquisition of the MS/MS spectra of isotopic ions of MH+ and (M + 3)+ with normal oxygen and (18)O at the alpha-carboxyl group of a partly (18)O-labeled peptide, which can be easily prepared by enzymatic hydrolysis of a protein in buffer containing 40 atom % H2(18)O. MS/MS analysis of an (18)O-labeled peptide by the present system allowed facile and reliable assignment of MS/MS product ions to a peptide sequence. The usefulness of the method was also demonstrated by measurement of some peptides that give MS/MS product ions incidentally observed at the same mass or assignable to some incorrect sequence.

Amino Acid Sequence↗
PubMed2001

Detection of tyrosine phosphorylated peptides by precursor ion scanning quadrupole TOF mass spectrometry in positive ion mode.

Phosphorylation is a common form of protein modification. To understand its biological role, the site of phosphorylation has to be determined. Generally, only limited amounts of phosphorylated proteins are present in a cell, thus demanding highly sensitive procedures for phosphorylation site determination. Here, a novel method is introduced which enables the localization of tyrosine phosphorylation in gel-separated proteins in the femtomol range. The method utilizes the immonium ion of phosphotyrosine at m/z 216.043 for positive ion mode precursor ion scanning combined with the recently introduced Q2-pulsing function on quadrupole TOF mass spectrometers. The high resolving power of the quadrupole TOF instrument enables the selective detection of phosphotyrosine immonium ions without interference from other peptide fragments of the same nominal mass. Performing precursor ion scans in the positive ion mode facilitates sequencing, because there is a no need for polarity switching or changing pH of the spraying solvent. Similar limits of detection were obtained in this approach when compared to triple-quadrupole mass spectrometers but with significantly better selectivity, owing to the high accuracy of the fragment ion selection. Synthetic phosphopeptides could be detected at 1 fmol/microL, and 100 fmol of a tyrosine phosphorylated protein in gel was sufficient for the detection of the phosphorylated peptide in the unseparated digestion mixture and for unambiguous phosphorylation site determination. The new method can be applied to unknown protein samples, because the identification and localization of the modification is performed on the same sample.

Amino Acid Sequence↗
PubMed1989

A "screened" electrostatic ion trap for enhanced mass resolution, mass accuracy, reproducibility, and upper mass limit in Fourier transform ion cyclotron resonance mass spectrometry.

Until now, it was thought that the optimal static electromagnetic ion trap for Fourier transform ion cyclotron resonance (FT-ICR) mass spectrometry should be designed to produce a quadrupolar electrical potential, for which the ion cyclotron frequency is independent of the ion's preexcitation location within the trap. However, a quadrupolar potential results in a transverse (to the magnetic field) electric field that increases linearly with distance from the center of the trap. That radially linear electric field shifts the observed ICR frequency, increases the ICR orbital radius, and ultimately limits the highest mass-to-charge ratio ion that can be contained within the trap. In this paper, we propose a new static electromagnetic ion "trap" in which grounded screens placed just inside the usual "trapping" plates produce a good approximation to a "particle-in-a-box" potential (rather than the quadrupolar "harmonic oscillator" potential). SIMION calculations confirm that the electric potential of the screened trap is near zero almost everywhere within the trap. For our screened orthorhombic (2.5 in. X 2 in. X 2 in.) trap, the experimental ICR frequency shift due to trapping voltage is reduced by a factor of approximately 100, and the experimental variation of ICR frequency with ICR radius is reduced by a factor of approximately 10 compared to a conventional (unscreened) 2-in. cubic ion trap.(ABSTRACT TRUNCATED AT 250 WORDS)

Electricity↗