Fast atom bombardment mass structure

In line with the policy of Advances to provide periodic coverage of major developments in physical methodology for the study of carbohydrates, A. Dell (London) here surveys the use of fast-atom-bombardment mass spectrometry in application to carbohydrates. This technique has achieved rapid prominence as the soft ionization technique of choice for structural investigation of complex carbohydrate sequences in biological samples. The author s extensive personal involvement in this field makes her chapter a critical, state-of-the-art overview for the specialist, as well as a valuable primer for the reader unfamiliar with this technique. 

A novel pigment has been isolated from the petals of Rosa hybrida with complex chromatographic techniques and the structure was elucidated with spectroscopic methods and high resolution fast-atom bombardement mass spectrometry, lH NMR, and FTIR. Anthocyanins were extracted from 7.9 kg of petals of Rosa hybrida cv. M me Violet with 80 per cent aqueous ACN containing 0.1 per cent TFA. The extract was purified in a Sephadex LH-20 column, and the fraction eluted with 80 per cent ACN was further fractionated in a HP-20 column using water, 15, 20 and 30 per cent ACN as mobile phases. The last fraction was lyophilized and separated by preparative RP-HPLC using an ODS column (50 X 5 cm i.d.). Solvents were 0.5 per cent aqueous TFA (A) and water-methanol... 

The low-resolution mass spectrum of Indinavir sulfate was measured using fast atom bombardment mass spectrometry on a JEOL HXl lOA mass spectrometer set at a resolution of 5000. The sample was ionized from a 5 1 dithiothreitol dithioerythritol matrix using xenon as the FAB gas. The low-resolution mass spectrum [12] ofindinavir is shown in Figure 14, while the structures of the structurally significant fragment ions are illustrated in Figure 15. 

The structures of the novel ferrocenyl dendrimers 1-6 were straightforwardly established by a variety of spectroscopic and analytical techniques including H, C, and Si NMR and IR spectroscopies, fast atom bombardment mass spectrome-... 

The structures of 294-296 have been resolved unambiguously by fast atom bombardment mass spectrometry and 1FI-, 13C- and 19F- NMR spectroscopic studies316. 

Fast atom bombardment mass spectrometry (FABMS) has become an important addition to the ionization techniques available to the analytical chemist in recent years. It has been particularly useful in a number of diverse applications which include molecular weight determinations at high mass, peptide and oligosaccharide sequencing, structural analysis of organic compounds, determination of salts and metal complexes, and the analysis of ionic species in aqueous solutions. This paper will focus on some aspects of the quantitative measurement of ionic species in solution. The reader is referred to a more comprehensive review for more details of some of the examples given here as well as other applications (1). 

A. Dell, H. R. Morris, H. Egge, H. von Nicolai, and G. Strecker, Fast-atom-bombardment mass spectrometry for carbohydrate structure determination, Carbohydr. Res., 115 (1983) 41-52. 

W. S. York, H. van Halbeek, A. G. Darvill, and P. Albersheim, Structural analysis of xyloglu-can oligosaccharides by H-n.m.r. spectroscopy and fast-atom-bombardment mass spectrometry, Carbohydr. Res., 200 (1990) 9-31. 

Single-crystal X-ray crystallography remains the only definitive technique for the structural characterization of heteronuclear gold cluster compounds, although other techniques, in particular Mossbauer, NMR, IR, and fast atom bombardment mass spectroscopies (FABMS), have yielded valuable information, especially concerning the nature of these species in solution. Electron spectroscopy, which has proved to be of great value in the identification of homonuclear gold cluster compounds (210) has received little attention by workers in this area,... 

References are given for spectroscopic studies, other v,c-oi IR hen these studies are reported in the synthetic/structural reference no further reference number is given. MS, mass spectrum FABMS, fast atom bombardment mass spectrum VT, variable-temperature. 

The characteristic H(4)-H(5) H NMR coupling constants of the 3-oxabicyclo[3.2.0]heptane derivatives anti-% (V//,//=1.3 Hz) and ry -51 Jh,h = 5.6 Hz) have been used to establish the structural assignments for these isomers <20060L491>. The structure of the rearranged cembrane derivative ciereszkolide 52 has been elucidated by onedimensional (TD) and 2-D NMR spectra, high-resolution fast atom bombardment mass spectrometry (HRFAB-MS), infrared (IR), and ultraviolet (UV) as well as by single crystal X-ray analysis <2004EJ03909>. 

S. Murao, K.Tanaka, and I. Nojima, Primary structure of paim I, an alpha-amylase inhibitor from Streptomyces corchorushii, determined by the combination of Edman degradation and fast atom bombardment mass spectrometry, Biochemistry 26 (1987), 6483-6488. 

This synthetic investigation confirmed the structure of the metabolite by comparison of fast atom bombardment-mass spectrometry (FAB-MS) spectra for the natural and synthetic cyclostellettamine C and for the monomeric synthetic compound 80 obtained by cyclization as indicated in Fig. (27). Additional confirmation came by comparing the bioactivities shown by synthetic dimer 55, mono-pyridinium 80 and natural cyclostellettamine C as antagonist agents for muscarinic receptors [43]. 

W. L. Roberts, S. Santikam, V. N. Reinhold, and T. L. Rosenberry, Structural characterization of the glycoinositol phospholipid membrane anchor of human erythrocyte acetylcholinesterase by fast atom bombardment mass spectrometry,./. Biol. Chem., 263 (1988) 18776—18784. 

Mass spectrometry can give valuable information on the structural details of Sn(II) heterometallic derivatives, subject to stability with respect to the disproportionation reaction in the vapor phase. The mass spectral results demonstrate that fast atom bombardment mass spectrometry (FARMS) could find immense applications in the characterization of heterometallic derivatives, particularly of non-volatile, high molecular weight compounds, such as those of tin. 

Figure 7). It should be emphasized that these quatemlzed glucuronldes are not minor metabolites and are particularly abundant In human urine, often representing more than 25X of the applied dose ( ). Quaternary I -glucuronldes can be synthesized by rabbit hepatic UDPGA transferase (57) and fast-atom bombardment mass spectrometry Is useful In structure Identifications (57,53) ... 

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