Secondary ion mass spectrometery: A new analytical technique for biologically important compounds

Benninghoven, A.; Sichtermann, W.

doi:10.1002/oms.1210120914

Cited by 124 publications

(29 citation statements)

References 3 publications

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“…Finally, as the above analysis would not distinguish between the two different forms of pyridinoline that have been reported [4], a mass spectrum was determined. TOF-SIMS proved to be eminently suitable for this, because of its high sensitivity (picomol to femtomol range) [16], applicability to thermally labile and nonvolatile compounds [17] such as the strongly polar cross-linking structures discussed here and the relatively simple spectra produced. It should also be noted that a mass spectrum alone is insufficient to characterise a cross-linking structure.…”

Section: Discussionmentioning

confidence: 99%

Characterisation of a type‐I collagen trimeric cross‐linked peptide from calf aorta and its cross‐linked structure

Henkel¹,

Glanville

Greifendorf

1987

European Journal of Biochemistry

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A collageneous trimeric cross-linked peptide has been isolated from the insoluble matrix of calf aorta, using trypsin solubilisation, and purified by gel filtration, cation-exchange chromatography and reversed-phase HPLC. Molecular mass and amino acid composition indicated that the C-terminal, non-helical region of type I collagen in its dimer form, designated as [Colc(I)]z, is cross-linked to a tryptic peptide TN(1) from the N-terminal helical cross-link region of an adjacent type I molecule, forming the cross-linked peptide [Colc(I)]z x TN(I).Amino acid sequence analysis of the peptide yielded a series of sequences corresponding to the cross-linking domains Colc(I) and TN(1) and furnished the first direct chemical evidence for the 4D staggered arrangement of type I molecules within native fibers.The trifunctional cross-linking amino acid pyridinoline was shown to occur in the peptide, confirming the peptides three-chain structure. Pyridinoline was isolated from the cross-linked peptide by preparative amino acid analysis and reversed-phase HPLC and identified by (a) its ultraviolet absorption spectra, (b) its fluorescence excitation and emission spectra and, for the first time, (c) its time-of-flight secondary ion-mass spectrum. The high sensitivity of the latter method, exceeding that of fast-atom-bombardement mass spectroscopy by three orders of magnitude, allowed detection of pyridinoline in the picomole range.The occurrence of pyridinoline in non-stoichiometric amounts, the presence of hydroxylysine in hydrolysates of all cross-linked peptides and the finding that hydrolysates also contained an unidentified component indicated that there is at least one cross-link form that is different from pyridinoline and is hydrolysable.It has been known for many years that the number of borohydride-reducible difunctional cross-links, present in fetal and young connective tissues, decreases markedly with age. It was suspected that the cross-links reacted further to give an altered cross-linking structure that was no longer reducible. This idea was supported by the characterisation of several trimeric collageneous cross-linked peptides which contained trifunctional cross-linking structures that were nonreducible [l, 21. It is only recently, however, that the Correspondence to W. Henkel, Institut fur Arterioskleroseforschung an der Universitat Miinster, DomagkstraDe 3, D-4400 Miinster, Federal Republic of Germany Abbreviation. TOF-SIMS, time-of-flight secondary ion-mass spectroscopy.Trivial name. Pyridinoline, the chemical structure is shown in Fig. 7.Nomenclature. [TC(I)l2 x TN(1) is a cross-linked peptide containing three polypeptide chains derived from a t ( [ ) of type I collagen. Tc(I) is the trypsin-derived peptide containing the carboxy-terminal nonhelical region of type I collagen. [Tc(I)l2 denotes the dimer of Tc(I). TN (1) detailed structures of such cross-links have been characterised. These nonreducible cross-links, among which pyridinoline is the best established compound, have been isolated from several tis...

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Section: Discussionmentioning

confidence: 99%

Characterisation of a type‐I collagen trimeric cross‐linked peptide from calf aorta and its cross‐linked structure

Henkel¹,

Glanville

Greifendorf

1987

European Journal of Biochemistry

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“…7 The appearance of molecular secondary ions in mass spectra of large organic molecules was a completely unexpected result that was first observed in studies of the secondary ion emission of amino acids deposited on metal surfaces by . 8 This work also demonstrated that the detection of large molecular species can be enhanced through metal cationization. Deposition of amino acids onto etched silver substrates resulted in the emission of secondary ions that consisted of amino acid molecules with silver ions attached.…”

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confidence: 81%

Static SIMS studies of carboxylic acids on gold and aluminium–magnesium alloy surfaces

Miller

Sun

Walzak

et al. 2003

Surface & Interface Analysis

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Static secondary ion mass spectrometry was used to study the surface reactions and lateral distributions of fatty carboxylic acid molecules on sputter-deposited gold and aluminium surfaces, as well as commercial aluminium-magnesium alloy surfaces, cleaned using UV/ozone. Films were prepared by spin coating dilute solutions of stearic acid and lauric acid onto the above surfaces. These carboxylic acids were shown to react with the oxide formed on the aluminium and aluminum-magnesium alloy substrates to produce a deprotonated acid anion, stabilized by the formation of a magnesium soap on the aluminium-magnesium alloy surface. Secondary ion imaging of stearic acid films revealed the formation of C-type crystals. Copyright  2003 John Wiley & Sons, Ltd. KEYWORDS:ToF-SIMS; carboxylic acids; aluminium-magnesium alloys; magnesium soap formation; C-type crystals Traditionally, mass spectrometry of organic molecules such as carboxylic acids has involved the introduction of the sample of interest into a heated ionization chamber, followed by the measurement of the mass to charge ratio using mass analysers such as quadrupoles, magnetic sector fields and time-of-flight tubes.1 The development of static secondary ion mass spectrometry by Benninghoven 2 has since allowed researchers to generate gas-phase ions from a solid surface containing species of high molecular mass, such as single layers of long-chain organic molecules held on a solid substrate.The study of organic molecules on surfaces using traditional instrumentation, such as x-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES), has not developed as rapidly as areas that are considered to be inorganic in nature, 3 such as the study of crystalline metal oxides. Progress in these areas has been hindered by the knowledge that organic thin films are often damaged by electron bombardment used for charge neutralization, they become unstable under high vacuum conditions or undergo charge shifting due to an electrically insulating nature. Techniques such as static SIMS and XPS have been used to confirm the damaged structures that arise when molecules of an organic film are subjected to severe x-ray or electron bombardment inside a spectrometer. Studies indicate that the damage induced is primarily due to photon-induced electrons that cause bond cleavage. 4 -6 Static SIMS, by contrast, uses a gentle ionization technique that can provide information about the surface chemistry of the outermost layers of a material while causing Ł Correspondence to: D. J. Miller, Surface Science Western, Western Science Centre, University of Western Ontario, London, Ontario, Canada N6A 5B7. E-mail: dmiller3@uwo.ca negligible surface damage. In general, static SIMS involves the use of mass spectrometry to measure the mass to charge ratio of secondary ions emitted from a solid surface when bombarded with a primary ion beam. The positively and negatively charged secondary ions emitted from the surface due to bombardment of the primary ion beam contain both elemental and m...

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“…It was designed for molecular surface analysis, where artifacts produced by the primary beam must be minimized to preserve the molecular information. Mass spectra of nonvolatile and/or thermally labile organic and biological molecules were obtained in this way (11,12).…”

Section: The Ion Emission Processmentioning

confidence: 99%

Liquid matrices for secondary ion mass spectrometry

Pauw¹

1986

Mass Spectrometry Reviews

122

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Secondary ion mass spectrometery: A new analytical technique for biologically important compounds

Cited by 124 publications

References 3 publications

Characterisation of a type‐I collagen trimeric cross‐linked peptide from calf aorta and its cross‐linked structure

Characterisation of a type‐I collagen trimeric cross‐linked peptide from calf aorta and its cross‐linked structure

Static SIMS studies of carboxylic acids on gold and aluminium–magnesium alloy surfaces

Liquid matrices for secondary ion mass spectrometry

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