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  • 1
    Electronic Resource
    Electronic Resource
    Analysis of native neutral glycosphingolipids by combined high performance liquid chromatography/mass spectrometry (1987)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 14 (1987), S. 149-153 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conditions for normal phase high performance liquid chromatrography-chemical ionization mass spectrometry of underivatized glycosphingolipids with the use of a moving belt transport interface were investigated. Chromatography was performed on a 2 mm ID × 3 cm column packed with 5 μm spherical silica. A gradient of increasing methanol and water in methylene chloride was used to resolve mono-, di-, tri-, and tetraglycosylceramides and sulfatides in less than 15 min. A polyimide belt was used to transport the sample residues to the mass spectrometer where ammonia chemical ionization mass spectrometry was used to obtain spectra. One to 5 μg of each component was sufficient to obtain full spectral scans. Mono- and dihexosylceramide spectra showed [M + H]+ ions of good abundance, while the higher glycosphingolipids have molecular weights that exceed the range of the mass spectrometer utilized. All glycosphingolipids gave ions characteristic of their ceramide, fatty acid, long chain base and carbohydrate components. Sequence information which reflected the relative position of hexose and N-acetylhexosamine residues was also obtained.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200140403
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  • 2
    Electronic Resource
    Electronic Resource
    Quantitative analysis of selected PCB congeners in marine matrix reference materials using a novel cyanobiphenyl stationary phase (1995)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 89-96 
    Details
    ISSN: 0935-6304
    Keywords: GC ; Stationary phases ; Cyanobiphenyl phase ; Polychlorinated biphenyls ; Reference Materials ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel p,p-cyanobiphenyl stationary phase (p-cyanobiphenyl, p-allyloxy methylpolysiloxane) has been evaluated for the GC investigation of polychlorinated biphenyls (PCBs). Several PCB congeners which coelute on the phases typically used for PCB analysis (e.g. 5% phenyl methylpolysiloxane) are separated on the p,p-cyanobiphenyl phase, including the hexachlorobiphenyl congeners PCB 163, PCB 164, and PCB 138. In this work, a p,p-cyanobiphenyl stationary phase was used to measure selected PCB congeners in two Standard Reference Materials (SRMs) available from the National Institute of Standards and Technology (NIST), and two Certified Reference Materials (CRMs) available from the Community Bureau of Reference (BCR). The materials analyzed were SRM 1588, Organics in Cod Liver Oil; SRM 1945, Organics in Whale Blubber; CRM 349, Chlorobiphenyls in Cod Liver Oil; and CRM 350, Chlorobiphenyls in Mackerel Oil. Concentrations are reported for several PCB congeners which coelute on the 5% phenyl methylpolysiloxane, including PCB 163 and PCB 164.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240180204
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  • 3
    Electronic Resource
    Electronic Resource
    Selected-ion accumulation from an external electrospray ionization source with a fourier-transform ion cyclotron resonance mass spectrometer (1993)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 7 (1993), S. 914-919 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The coupling of an electrospray ionization (ESI) source to a Fourier-transform ion cyclotron resonance (FTICR) mass spectrometer provides a facility for the high resolution, accurate mass analysis of large biopolymers. Typically the m/z range of the electrosprayed ions injected and trapped in the FTICR cell is between m/z 500 and 2500 (but can vary considerably with solution conditions). Recent reports on quadrupole excitation have demonstrated the ability to cool the magnetron motion of ions trapped in the FTICR mass spectrometer cell by converting this motion to cyclotron motion which, under appropriate pressure conditions, damps readily to the center of the cell. The use of a broadband waveform (swept frequency or stored waveform inverse Fourier-transform) for the quadrupole cooling pulse was shown to provide cooling of a wide range of m/z ions, while implementation of a single frequency demonstrated a much narrower m/z response. This report demonstrates the successful combination of single-frequency quadrupole cooling with external injection of electrosprayed ions into an FTICR mass spectrometer for m/z selected-ion accumulation. This capability is particularly significant with electrospray ionization since it allows ions of only one charge state to be accumulated in the cell, and greatly increases the potential dynamic range of ESI-FTICR.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290071012
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  • 4
    Electronic Resource
    Electronic Resource
    Time-base modulation for the correction of cyclotron frequency shifts observed in long-lived transients from fourier-transform ion-cyclotron-resonance mass spectrometry of electrosprayed biopolymers (1993)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 7 (1993), S. 700-703 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The occurrence of small shifts in the cyclotron frequency during the acquisition of very long transients (in excess of 80 s) has been observed to be a limiting factor for ultrahigh-resolution mass measurements of protein ions performed with electrospray-ionization Fourier-transform ion-cyclotron-resonance mass spectrometry. Resolution measurements were restricted to values less than 106 because of the frequency shifts. Measurements of the frequency shifts, performed by sequentially transforming small segments of the transient, allowed the shift to be characterized and fitted to a 4th-order equation. The sampling rate of the acquired transient was then modulated (at a rate equal to the reciprocal of the rate for the frequency shift) to allow ultrahigh resolution, greater than 2 × 106, and improved mass measurement and precision to be achieved for a small protein.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290070803
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  • 5
    Electronic Resource
    Electronic Resource
    Measurement of plasma free fatty acid turnover and oxidation using [1-13C]palmitic acid (1980)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1980), S. 168-171 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The measurement of plasma free fatty acid turnover and oxidation by means of the isotopic dilution technique using a radiolabeled free fatty acid has proven useful for the in vivo study of fat metabolism in animals. However, because of the ethical considerations regarding the administration of radioisotopes to humans, there is a lack of adequate information regarding the in vivo regulation of free fatty turnover and oxidation in humans, particularly children. Consequently, we have developed a technique using the stable, nonradioactive [1-13C]palmitic acid molecule as free fatty acid tracer to measure plasma free fatty acid metabolism in vivo. We have analysed the isotopic enrichment of plasma palmitate by selected ion monitoring on a gas chromatograph mass spectrometer and we have used an isotope ratio mass spectrometer to determine the much lower isotopic enrichment of the expired CO2. We have found this technique to be safe to administer, to have a high degree of analytical reproducibility, and to yield values in dogs comparable with those obtained using [1-14C]palmitic acid as the tracer.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200070407
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  • 6
    Electronic Resource
    Electronic Resource
    The construction and use of simple interfaces for combined liquid chromatography mass spectrometry (1981)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 316-321 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This paper describes the development of two easily constructed, inexpensive interfaces for combined liquid chromatography mass spectrometry. The first interface directly introduces a small percentage of liquid chromatographic eluent into the ion source of the mass spectrometer, whilst the second employs vacuum nebulization to vaporize sample and solvent. Both interfaces have been designed as removable probes. The construction and operation of the interfaces are discussed in detail and a comparison of their performance is made. Examples of the application of liquid chromatography mass spectrometry to the determination of low levels of specific components in complex matrices are given.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200080707
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  • 7
    Electronic Resource
    Electronic Resource
    Use of a microchannel array detector in a four-sector tandem mass spectrometer (1988)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1988), S. 147-151 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200170214
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  • 8
    Electronic Resource
    Electronic Resource
    Bio-affinity characterization mass spectrometry (1995)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 9 (1995), S. 644-650 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A new approach, bio-affinity characterization mass spectrometry (BACMS), aimed at providing a more rapid, sensitive and potentially more flexible alternative to techniques presently employed for the characterization of noncovalent interactions in mixtures, such as would be encountered in combinatorial chemistry, is presented. BACMS avoids some of the difficulties and potential artifacts associated with affinity chromatography since the noncovalent associations occur in solution; thus, BACMS avoids the requirement of solid support media and the development of non-interfering linker species. This paper describes the conceptual basis for the methodology and its potential use in applications which include the screening of high affinity ligands in support of new drug development. BACMS exploits new Fourier-transform ion cyclotron resonance (FTICR) mass spectrometry technologies which, when coupled to electrospray ionization (ESI), allow the investigation of specific noncovalent complexes formed in solution. BACMS utilizes the well-known attributes of FTICR, such as the high resolution mass analysis and (MS)n (n ≥ 2) capabilities; however, it is even more directly a result of recently developed techniques involving quadrupolar excitation, such as selected-ion accumulation. These tools are demonstrated and the results illustrate the extraordinary sensitivity achievable (solution concentrations of 1 × 10-9 M without the use of separations prior to ESI). Thus, the new capabilities demonstrated here, in conjunction with ESI, will be useful for the investigation of very low relative concentration noncovalent association directly from solution, and promote a faster alternative for combinatorial mixture screening and analysis.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290090805
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  • 9
    Electronic Resource
    Electronic Resource
    Comparison of selectivities for PCBs in gas chromatography for a series of cyanobiphenyl stationary phases (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 221-230 
    Details
    ISSN: 1040-7685
    Keywords: gas chromatography ; stationary phases ; cyanobiphenyl phasesshape selectivity ; polychlorinated biphenyls ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selectivity for polychlorinated biphenyl (PCB) congeners was examined for a series of cyanobiphenyl stationary phases, and the results were compared to a nonpolar 5% phenyl methylpolysiloxane phase and a shape-selective smectic liquid crystalline phase. For all of the columns studied, the degree of ortho substitution of the congener was found to be a significant factor controlling chromatographic retention of PCBs. The retention pattern on six different cyanobiphenyl phases followed the same general pattern as on the liquid crystalline column, though the trends were more exaggerated on the liquid crystalline phase. While the general retention pattern was similar for all of the cyanobiphenyl phases studied, subtle differences were observed, resulting in significant selectivity differences. For isomeric planar PCB congeners, elution order could be correlated to length-to-breadth ratios. Among the cyanobiphenyl phases, the p,p- and the o,p,p-cyanobiphenyl phases had the greatest enhancement of retention for planar congeners. A shapeselective test mixture reflected the similarity of retention on the cyanobiphenyl phases to both the 5% phenyl methylpolysiloxane phase and the smectic liquid crystalline phase. © 1995 John Wiley & Sons, Inc.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220070306
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  • 10
    Electronic Resource
    Electronic Resource
    Screening techniques for the detection of inborn errors of bile acid metabolism by direct injection and micro-high performance liquid chromatography-continuous flow/fast atom bombardment mass spectrometry (1993)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 22 (1993), S. 331-337 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two methods, direct injection-continuous flow fast atom bombardment (DI-CF/FAB) mass spectrometry and micro-high-performance liquid chromatography (μHPLC)-CF/(FAB) mass spectrometry were developed for the clinical analysis of urinary bile acids and their conjugates, specifically for the diagnosis of disorders of bile acid metabolism. The method based upon DI of urine extracts into the CF/FAB flow stream was developed for the rapid screening of large numbers of patient samples. It allows injections to be made at 4 min intervals for high sample throughput. Analyses of standard mixtures of bile salts demonstrate that linear response curves are obtained over more than a hundred-fold concentration range with a minimum detectable amount in the picogram range. Oxo bile salts are identified by reduction with sodium borodeuteride followed by reanalysis for detection of any reduction products. This methodology has been used for the analysis of over 1000 specimens. A reverse-phase μHPLC-CF/FAB mass spectrometric method was also developed for use in the confirmation or further investigation of screening results. With no additional sample preparation this method permits the separation, identification and quantitation of urinary bile salt isomers within a 45 min analysis time.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200220604
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