Metal isotope coded profiling of organic ligands by mass spectrometry in aquatic environments
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AbstractMass spectrometry is a powerful analytical tool for determining the isotope ratios and concentrations of trace elements in various samples at levels ranging from major constituents to subparts per billion. Because isotope dilution is free from matrix effects, it has the potential of being incorporated into a definitive analytical approach that can provide reference values for concentrations in physiological and pathological conditions. In addition, isotope dilution mass spectrometry results are free from the constraints of quantitative recovery of the analyte, an essential requirement in other analytical techniques that is difficult to achieve with complex biological samples. A variety of mass spectrometric approaches have been used for determining the concentration of trace elements in biological samples. The more commonly used are thermal ionization mass spectrometry, inductively coupled plasma mass spectrometry, fast atom bombardment mass spectrometry, and gas chromatography mass spectrometry. This article reviews the work on trace element determination in biological samples using different mass spectrometric techniques and highlights the experiments performed by the authors in establishing gas chromatography mass spectrometry.Key Words:: gas chromatography-mass spectrometryfast atom bombardment-mass spectrometryinductively coupled-plasma mass spectrometrythermal ionization-mass spectrometryisotope dilutionbiological samplesmatrix effectstrace elements
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Rationale To achieve better precision and accuracy for delta C-13 analysis of individual amino acids (AAs), we have developed a new analytical method based on multi-dimensional high-performance liquid chromatography (HPLC) and elemental analyzer/isotope ratio mass spectrometry (EA/IRMS). Unlike conventional methods using gas chromatography, this approach omits pre-column chemical derivatization, thus reducing systematic errors associated with the isotopic measurement. Methods The separation and isolation of individual AAs in a standard mixture containing 15 AAs and a biological sample, spear squid (Heterololigo bleekeri) were performed. AAs were isolated using an HPLC system equipped with a reversed-phase column and a mixed-mode column and collected using a fraction collector. After the chromatographic separation and further post-HPLC purification, the delta C-13 values of AAs were measured by EA/IRMS. Results The complete isolation of all 15 AAs in the standard mixture was achieved. The delta C-13 values of these AAs before and after the experiment were in good agreement. Also, 15 AAs in the biological sample,H. bleekeri, were successfully measured. The delta C-13 values of AAs inH. bleekerivaried by as much as 30 parts per thousand with glycine being most enriched in(13)C. Conclusions The consistency between the delta C-13 values of reference and processed AAs demonstrates that the experimental procedure generates accurate delta C-13 values unaffected by fractionation effects and contamination. This method is therefore suitable for delta C-13 analysis of biological samples with higher precision than conventional approaches. We propose this new method as a tool to measure delta C-13 values of AAs in biological, ecological and biogeochemical studies.
Isotope dilution
Isotope-ratio mass spectrometry
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The sediment of the Charles River Basin (an exclusively anaerobic system) was analyzed by computerized gas chromatographic-mass spectrometry (GC-MS) and high resolution mass spectrometry (HRMS). The organic compounds were separated first by methylene chloride extraction followed by gradient chromatography on alumina. This analysis revealed a large number of aliphatic and olefinic hydrocarbons, elemental sulfur, various and abundant polycyclic aromatic hydrocarbons (PCAH) and their alkyl derivatives, and two phthalate esters. Since the PCAH were the most abundant single class of compounds, their identification was pursued in detail. Possible sources of these compounds in the aqueous environment are petroleum, incomplete combustion, anaerobic biosynthesis, or chemical dehydrogenation of natural products.
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Abstract Compound-specific isotope analysis of 15N enrichment of nitrogenous molecules by gas chromatography/isotope ratio mass spectrometry is a potential method for a quantitative access of nitrogen flow in plant nutrition and biosynthesis. Here, as a primary application of this method for plant nutrition studies, we demonstrate high sensitive detection of 15N enrichment of amino acids in white radish cultivated either with very low level of 15N-labeled organic or inorganic nutrients, and evaluate the practical utility of this method.
Isotope-ratio mass spectrometry
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A method is described for the chemical purification and mass spectrometry of the enriched 10B and 11Bthat are separated by the electromagnetic method, and some measures are taken for increasing the analytical sensitivity and the stabilization of the ion beam in the isotope mass spectrometry of micro amount of solid boron.
Isotopes of boron
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