Phytoecdysteroid analysis by high-performance liquid chromatography-thermospray mass spectrometry
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Thermospray
Ecdysteroid
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Repeatability
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Atmospheric-pressure chemical ionization
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Hybrid mass spectrometer
Quadrupole mass analyzer
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Ion-mobility spectrometry–mass spectrometry
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During the past several years, mass spectrometry has made great progress in the analytical field of biological molecules. The progress has been mainly achieved with the development of new soft ionization techniques, such as plasma desorption, laser desorption, molecular secondary ion mass spectrometry, and fast atom bombardment mass spectrometry, and with the development of a big mass spectrometer. It has been demonstrated that polar nonvolatile big bioorganic molecules can be ionized without dissociation by soft ionization methods, which are called desorption ionization. The soft ionization methods and recent applications are overviewed. Newly developed thermospray ionization seems to be obtaining a reputation as a suitable ionization method for LC/MS and several applications have been achieved more recently. The application of tandem mass spectrometry (MS/MS) to structure analysis or mixture analysis of bioorganic samples has started recently, while it was widely used as a method for analyzing the ion structure of small molecules. These combination techniques of using a mass spectrometer with a liquid chromatograph or another mass spectrometer are promising methods for mixture analysis and they are also reviewed here.
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Ambient ionization
Desorption electrospray ionization
Fast atom bombardment
Field desorption
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Thermospray
Isobutane
Fast atom bombardment
Atmospheric-pressure chemical ionization
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Abstract Complex formation between different polyols, carbohydrates and borate was studied by thermospray mass spectrometry. The analytes were dissolved in 0.1 M ammonium borate buffer and introduced through a standard thermospray interface into a quadrupole mass spectrometer. The formation of various complexes which gave rise to relatively abundant ions in the thermospray spectra was observed. A correlation has been found between the relative intensities of these ions and the orientation of the hydroxyl groups involved in the complexation.
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This study demonstrates a useful application of on-line microbore high-performance liquid chromatography (HPLC) fast atom bombardment (FAB) and thermospray (TSP) mass Spectrometry techniques for identification of metabolites from the in vitro metabolism of an experimental Monsanto herbicide: 2-chloro-N-(ethoxymethyl-N-[2-methyl-6-(trifluoromethyl) phenyl]acetamide), ‘chloroacetanilide’. The microbore HPLC FAB technique on a high-resolution sector mass spectrometer accelerated identification of polar metabolites from the in vitro metabolism study of the herbicide. It provided good chromatographic resolution and excellent FAB sensitivity with strong protonated molecular ions. Scanning high-resolution LC/FAB mass spectrometry also provided molecular formulae for structural elucidation of unknown metabolites. Sample purification and concentration were minimized. Identification of less polar metabolites was carried out using LC/TSP mass spectrometry with a quadrupole mass spectrometer. LC/TSP mass spectrometry provided useful structural information for both polar and less polar metabolites because their spectra showed more fragmentation than FAB spectra. Glutathione conjugation was the major reaction observed during in vitro incubation of the herbicide. Oxidation of the chloroacetanilide by rat liver enzymes was also a significant metabolic reaction. Seven metabolites were identified, of which four were glutathione conjugates.
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Fast atom bombardment
Fragmentation
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Ion-mobility spectrometry–mass spectrometry
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