Secondary ion mass spectrometry of protected diribonucleoside monophosphates with a time-of-flight mass spectrometer

Ens, Werner; Standing, Kenneth G.; Westmore, John B.; Ogilvie, Kelvin K.; Nemer, Mona J.

doi:10.1021/ac00243a028

Cited by 48 publications

(12 citation statements)

References 34 publications

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“…For example, field desorption (FD) (2, 3), desorption chemical ionization (DCI) (4), thermospray (5), and liquid ionization (6) have been successfully used for the analysis of nonderivatized nucleosides and nucleotides. More recently impressive results on polar, nonvolatile organic molecules have been demonstrated using a group of particle-induced desorption ionization techniques, e.g., secondary ion mass spectrometry (SIMS) (7,8), 252Cf plasma desorption mass spectrometry (PDMS) (9)(10)(11), laser desorption (LD) (12), and fast atom bombardment mass spectrometry (FAB-MS) (13)(14)(15)(16)(17)(18)(19)(20)(21)(22)(23)(24).…”

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confidence: 99%

Differentiation of isotopically labeled nucleotides using fast atom bombardment tandem mass spectrometry

Mallis¹,

Raushel²,

Russell³

1987

Anal. Chem.

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Differentiation of isotopically labeled nucleotides using fast atom bombardment tandem mass spectrometry

Mallis¹,

Raushel²,

Russell³

1987

Anal. Chem.

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“…If there is a kinetic isotope effect associated with the ionic fragmentaion (as there usually is) then these coefficients will not be equal ( a # /3). Substituting eq 10a and 10b into eq 9 for the mole fractions of the isotope variants of the split fragment ion, X V ) i k , and rearranging give the result Mi = MO + N;((mH -mL) + aM(n)L -PM(n)H} (11) where M (~) L and M (~) H represent the average masses for the neutral fragments eliminated in forming the light and heavy isotopic forms of the fragment ions. Note that since a and /3 are constants for a given material under a given set of experimental conditions, the collection of terms within the braces is also a constant.…”

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confidence: 99%

“…Since the solution to the average mass equation is direct and exact for compounds with complex naturally occurring isotopic distributions, this method may be ideally suited to the isotopic analyses of materials which contain polyisotopic elements (such as inorganic and organometallic compounds). Work in other laboratories has demonstrated that it is pmsible to measure the average mass of an isotopic cluster precisely even at high mass (8) and when the peaks in the cluster are not resolved (9)(10)(11). Consequently, the average mass approach could eventually prove useful in the isotopic analyses of high molecular weight samples and those which require the use of mass spectral methods which cannot provide unit mass resolution.…”

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“…Work in other laboratories has demonstrated that it is possible to measure the average mass of an isotopic cluster precisely even at high mass (8) and when the peaks in the cluster are not resolved (9)(10)(11). Consequently, the average mass approach could eventually prove useful in the isotopic analyses of high molecular weight samples and those which require the use of mass spectral methods which cannot provide unit mass resolution.…”

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Average mass approach to the isotopic analyses of compounds exhibiting significant interfering ions

Blom¹

1988

Anal. Chem.

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Kalinoski, H. T.; Udwth, H. R.; Smith, R. D. HRC CC, J.High Resolut. Chromatogr . Chromatogr . Commun . 1988, 9 , 145-153. 23. 192-199. . .of the oligosaccharides. The mode of splitless injection used in this work is a step toward making SFC-MS a quantitative, trace analysis technique. Injection technology being developed in a number of laboratories which will allow the splitless injection of solutes present in microliter volumes will strengthen the standing of SFC and SFC-MS in this area. Capillary supercritical fluid chromatography-mass spectrometry using an unmodified C02 mobile phase as presented here is limited to relatively nonpolar solutes. The use of modified and more polar mobile phases should extend the range of solute polarities which SFC-MS can handle (28). As the high-mass performance of quadrupole mass analyzers improves and as problems in interfacing SFC to mass spectrometer ion sources operating at high voltage are overcome ( 1 7 ) SFC-MS and SFI-MS will become even more powerful tools in characterizing mixtures containing high molecular weight, less volatile species. ACKNOWLEDGMENTStrife for guidance and useful discussions. The authors thank T. L. Chester, T. Keough, and R. J. Registry No. Methyl arachidate, 1120-28-1; tristearin, 555-43-1. LITERATURE CITED (1) Markides, K. E.; Fields, S. M.: Lee, M. L. J. Chromatogr. Sci. 1986, 2 4 , 254-257.(2) Chester, T. L.; Innis, D. P. HRC CC, J. High Resoluf. Chromatogr. Chromatogr. Commun. 1988, 9 , 209-212. (3) Gouw, T. H.; Jentoft, R. E.; Gallegos, E. J. J. High Pressure Scl. Techno/. AIRAPT Conf. 6th 1979, 583-592.

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“…We could not obtain protonation or deprotonation under any experimental conditions. Plasma desorption mass spectrometry has been shown by McNeal et al 13 and secondary ion mass spectrometry (SIMS) by Ens et d 3 and Beavis et all4 to have advantages in this area. Our next objective was to check out fully protected dinucleotides, where one of the protection groups is missing, namely the end phosphate, which is protected normally with tribromoethyl or cyanoethyl.…”

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Mass spectroscopic sequence analysis of oligonucleotides

Grotjahn

Blöcker

Frank

1985

Biol. Mass Spectrom.

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Negative ion fast atom bombardment (FAB) mass spectroscopy is used for sequencing fully deprotected oligonucleotides, 5'-tritylated oligonucleotides and negatively charged protected oligonucleotides. The mass spectrometric bidirectional sequence analysis allows characterization of modified oligonucleotides, even those where all classical sequencing methods have so far failed. Examples from each class of compound are illustrated and the problems and methodology are discussed. INTRODUCTION ~ ~Fast atom bombardment mass spectrometry is a suitable method for characterization of bio-oligomers.'-' Information is obtained not only about the molecular mass, but also about the structure from the many fragment ions. These fragments are generally formed by cleavage of bonds to heteroatoms. In the case of peptides this is at nitrogen and fragmentation allows sequence information in both positive and negative ion modes to be In the case of oligonucleotides cleavage occurs at oxygen which allows bidirectional sequence analysis for unprotected, negatively charged protected and modified oligonucleotides in the negative ion mode.678 DNA chemists have made considerable progress in the synthesis of various 'linker and adapter' molecules related to DNA. These compounds allow a vast number of new combinations of gene material to be produced. Other small fragments in the DNA molecule can be changed and synthetic material built in at the desired point in the molecule to give a mutation of natural DNA.The synthesis of these small DNA fragments can be performed in a matter of days and as a consequence the longer part of the work is now the careful analysis of the deprotected oligonucleotides.Previously these analyses, which involve checking the sequence of the synthetic material, have been performed by the often laborious methods of chemical degradation" or wandering spot techniques," involving radioactive labelling.The mass spectrometric bidirectional sequence analysis is less time consuming than any other sequencing procedure known to date.We use the latter method for oligonucleotides up to 10 base units, when ca. 1 OD is available. Sequence analysis by classical methods take approximately two days, while mass spectroscopic analysis requires approximately 1 hour. ~~ EXPERIMENTALThe FAB mass spectra were obtained on a KRATOS MSSO S with a high field magnet equipped with a t Author to whom correspondence should be addressed.KRATOS FAB source. The atom gun used xenon and produced a beam of neutral atoms at 8-9 kV. The spectra were recorded at a magnet scan rate of 300 s decade-'.Oligodeoxyribonucleotides were synthesized following, in general, the established phosphate triester pro~edure.,.~ Ribonucleotides were of commercial origin (P-L Biochemicals, Milwaukee, USA). UGUU was prepared enzymatically (generously provided by Reinhard Liihrmann, Max-Planck-Institut fur Molekulare Genetik, Berlin-Dahlem).Samples were prepared in various ways. A water solution of the triethylammonium salt of each oligonucleotide, (ca. 4 p,l, containing ca. 1 O...

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Secondary ion mass spectrometry of protected diribonucleoside monophosphates with a time-of-flight mass spectrometer

Cited by 48 publications

References 34 publications

Differentiation of isotopically labeled nucleotides using fast atom bombardment tandem mass spectrometry

Differentiation of isotopically labeled nucleotides using fast atom bombardment tandem mass spectrometry

Average mass approach to the isotopic analyses of compounds exhibiting significant interfering ions

Mass spectroscopic sequence analysis of oligonucleotides

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