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A selective and sensitive method for determination of total homocysteine (Hcy) in human serum, by gas chromatography coupled to ICP-MS(HR), has been developed. After reduction of the sample with sodium borohydride the liberated Hcy and other aminothiols, such as cysteine (Cys) and methionine (Met), were converted to their N-trifluoroacetyl (TFA)- O-isopropyl derivatives and these were injected into a gas chromatograph equipped with an HP-5 capillary column. Detection was carried out by means of a double-focusing inductively coupled plasma mass spectrometer (DF-ICP-MS) monitoring (32)S at m/Delta m (resolving power)=3000. The transfer line used to transport the analytes from the GC column to the ICP-MS had previously been developed in our laboratory. The different parameters affecting the derivatisation process were optimised, as were the instrumental operating conditions. This optimised GC-ICP-MS(HR) method was successfully applied to the determination of total homocysteine in human serum-values obtained were in agreement with data reported in the literature. Quantitative recoveries and good precision were obtained for spiked human serum, demonstrating the suitability of the method for quantitative determination of total homocysteine in serum.
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PMID:Determination of total homocysteine in human serum by capillary gas chromatography with sulfur-specific detection by double focusing ICP-MS. 1284 8

Variations in Hg isotope ratios in cinnabar ores obtained from different countries were detected by high precision isotope ratio measurements using multi-collector inductively coupled mass spectrometry (MC-ICP-MS). Values of delta198/202Hg varied from 0.0-1.3 percent per thousand relative to a NIST SRM 1641d Hg solution. The typical external uncertainty of the delta values was 0.06 to 0.26 percent per thousand. Hg was introduced into the plasma as elemental Hg after reduction by sodium borohydride. A significant fractionation of lead isotopes was observed during the simultaneous generation of lead hydride, preventing normalization of the Hg isotope ratios using the measured 208/206Pb ratio. Hg ratios were instead corrected employing the simultaneously measured 205/203T1 ratio. Using a 10 ng ml(-1) Hg solution and 10 min of sampling, introducing 60 ng of Hg, the internal precision of the isotope ratio measurements was as low as 14 ppm. Absolute Hg ratios deviated from the representative IUPAC values by approximately 0.2% per u. This observation is explained by the inadequacy of the exponential law to correct for mass bias in MC-ICP-MS measurements. In the absence of a precisely characterized Hg isotope ratio standard, we were not able to determine unambiguously the absolute Hg ratios of the ore samples, highlighting the urgent need for certified standard materials.
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PMID:High precision isotope ratio measurements of mercury isotopes in cinnabar ores using multi-collector inductively coupled plasma mass spectrometry. 1286 80

The HPLC-ICP-MS coupling technique is able to separate and detect methyl, ethyl and inorganic mercury isotopes specifically. An identification of ethyl mercury(+) is not possible when the widely used sodium tetraethylborate derivatisation method in combination with GC-AFS/AAS or ICP-MS techniques is performed because it contains ethyl groups.An unidentified compound with the same retention time as ethyl mercury was found in the HPLC chromatograms of industrial sewage samples and humic-rich soils of microcosm experiments after applying water vapour distillation. We also observed such unidentified peaks in samples of heavily contaminated sites in Eastern Germany, separated by HPLC fractionation only. In the experiments described, different mercury sulfur adducts were synthesised and tested for their retention times in the HPLC-ICP-MS system. It was found that the compound CH(3)-S-Hg(+) showed the same retention time as the ethyl mercury standard. It is therefore possible that ethyl mercury detected in chromatography by comparison of the retention time could also be due to an adduct of a sulfur compound and a mercury species. CH(3)-S-Hg(+ )should be tested in other chromatographic mercury speciation methods for this effect. This work can also be regarded as a contribution to the discussion of artificially occurring methyl mercury in sediments during sample preparation.
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PMID:Possible interferences of mercury sulfur compounds with ethylated and methylated mercury species using HPLC-ICP-MS. 1287 5

The Llobregat and Ter Rivers, typical Mediterranean catchments in Northeast Spain, supply water to more than 4.5 million inhabitants residing in the metropolitan area of Barcelona. The objective of this work is to study the factors that influence the surface water quality of Llobregat catchment. As such, spatial and temporal variations of more 50 water chemical parameters were monitored in 10 sampling sites for a period that extended from July 1996 to December 2000. The temperature, pH and conductivity were measured at sites, whereas metals were analysed using ICP-OES and ICP-MS instrumental techniques. The head waters of the Llobregat River catchment flow through detrital Mesozoic-Cenozoic sedimentary rocks resulting in calcium bicarbonate-type water with low mineral content. The high water quality of the waterhead is deteriorated in the upper-middle part of the catchment due to: occurrence of evaporite-bearing geological formations, and the mining and industrial activities related to potash exploitation. As a result, an obvious increase in Na, K, Mg, Cl-, Br, Rb, and Sr concentrations is reported leading to a sodium (potassium) chloride water type. This saline hydrochemical fingerprint persists downstream. This important feature renders the low water quality of the Llobregat River to be adequate for drinking supply purposes. In addition, the industrial and residential activities, specially at the lower part of the catchment, increases P, B, Mn, Fe, Pb, Al, Cr, Co, Ni, Cu, Zn, As and Sb water concentrations.
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PMID:Spatial and seasonal variations of water quality in a Mediterranean catchment: the Llobregat River (NE Spain). 1474 Sep 88

X-ray and time of flight neutron diffraction data, FTIR and MAS-NMR spectra, and ICP-AES and carbonate analyses have been collected from a sodium-containing carbonate apatite (CO(3) content 12.5(7)wt%). A structural model based on Holly Springs hydroxyapatite without CO(3)(2-) ions showed an apparent reduction in the PO(4) tetrahedral volume which is ascribed to CO(3)(2-) replacing PO(4)(3-) ions in the lattice. Four structural models from the literature with the CO(3)(2-) ion explicitly modelled were fitted to the neutron diffraction data by the Rietveld method. The best fit was obtained with the CO(3)(2-) ion in disorder between the mirror symmetry related faces of a vacant PO(4)(3-) site and with the normal to the plane of the CO(3)(2-) ion at approximately 30 degrees to the c-axis. This angle is consistent with results from previous polarised IR measurements on single crystals of francolite (a fluorocarbonate apatite) and human dental enamel. Further refinement of the model revealed a hitherto unknown atom site close to the unit cell origin, (possibly a water molecule). The refined hexagonal unit cell parameters from the neutron diffraction data were a=9.3446(3)A and c=6.9199(4)A.
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PMID:Rietveld structure refinement of precipitated carbonate apatite using neutron diffraction data. 1474 36

An approach for screening and resolving selenium-containing plant proteins was developed based on the combination of sample preparation and multi-dimensional liquid chromatography coupled to ICP-MS. Different protein extraction protocols were investigated. A 24 h dodecylsulfate-mediated protein extraction in a sonication bath followed by acetone precipitation was found to be optimal. The use of different protein precipitate solubilizing agents (sodium dodecyl sulfate media and Tris-HCl buffer) demonstrates possible fractionation of the selenium-containing proteins. Selenium-containing protein screening and fractionation were carried out by means of SEC-ICP-MS. High molecular weight selenium containing proteins were solubilized with a sodium dodecyl sulfate-containing buffer, whereas the low molecular weight compounds were released into a Tris-HCl buffer. Size exclusion chromatography-fast protein liquid chromatography coupled to ICP-MS allowed separation and detection of several selenium-containing proteins in Se-supplemented wild type Brassica juncea plant, a fast growing selenium accumulator.
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PMID:Preliminary studies on selenium-containing proteins in Brassica juncea by size exclusion chromatography and fast protein liquid chromatography coupled to ICP-MS. 1475 53

In this work, we studied the extraction of beta chitin from squid pens. The characterization by ICP of the raw material confirmed the significant absence of calcium carbonate and then the possibility to definitely avoid a step of demineralization responsible for chain degradation. The kinetics studies associated with the extraction of lipid parts showed the important role played by the latter structures on the limitation of the protein extraction by a simple treatment in an aqueous solution of 1 M NaOH. The role of various parameters such as the size of the particles, time and number of steps, and the concentration in sodium hydroxide was studied. The determination of the molecular characteristics (molecular weight and degree of acetylation) allowed us to define the optimal conditions of deproteinization in relation with the best preservation of these characteristics.
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PMID:New aspects of the extraction of chitin from squid pens. 1500 21

Suppressed conductimetric detection ion chromatography (IC) was investigated for the separation and detection of common inorganic anions, calcium and magnesium by anion-exchange chromatography using a sodium carbonate-EDTA mobile phase. The formation of anionic Ca2+ -EDTA and Mg2+ -EDTA complexes allowed its separation from other inorganic anions opening the way for their simultaneous determination in a single chromatographic run. The effect of the pH, carbonate and EDTA concentrations in the eluent and the previous addition of EDTA to the samples has been studied. The optimised experimental conditions were applied to the determination of Ca2+ and Mg2+ in mineral waters with results in agreement with alternative ICP-MS methodologies.
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PMID:Simultaneous determination of inorganic anions, calcium and magnesium by suppressed ion chromatography. 1507 97

A new method for the determination of nine haloacetic acids (HAAs) with ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was developed. With the very hydrophilic anion-exchange column and steep gradient of sodium hydroxide, the nine HAAs could be well separated in 15 min. After suppression with an ASRS suppressor that was introduced in between IC and ICP-MS, the background was much decreased, the interference caused by sodium ion present in eluent was removed, and the sensitivities of HAAs were greatly improved. The chlorinated and brominated HAAs could be detected as 35ClO and 79Br without interference of the matrix due to the elemental selective ICP-MS. The detection limits for mono-, di-, trichloroacetic acids were between 15.6 and 23.6 microg/l. For the other six bromine-containing HAAs, the detection limits were between 0.34 and 0.99 microg/l. With the pretreatment of OnGuard Ag cartridge to remove high concentration of chloride in sample, the developed method could be applied to the determination of HAAs in many drinking water matrices.
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PMID:Determination of trace-level haloacetic acids in drinking water by ion chromatography-inductively coupled plasma mass spectrometry. 1525 Apr 8

The root/organic soil concentration ratio; R/S) of 50 cationic mineral elements was related to their ionic properties, including ionic radius (r), ionic charge (z), and ionic potential (z/r or z2/r). The materials studied were ectomycorrhizal beech (Fagus sylvatica L.) roots and their almost purely organic soil substrate, the O-horizon (mor; raw humus) of a Podzol in South Sweden, developed in a site which has been untouched by forestry or other mechanical disturbance since at least 50 years and located in an area with no local sources of pollution. Elements determined by ICP-AES were aluminium, barium, calcium, iron, potassium, magnesium, manganese, sodium and strontium. Determined by ICP-MS were silver, beryllium, bismuth, cadmium, cerium, cobalt, chromium, caesium, copper, dysprosium, erbium, europium, gallium, gadolinium, hafnium, mercury, holmium, indium, lanthanum, lithium, lutetium, niobium, neodymium, nickel, lead, praseodymium, rubidium, scandium, samarium, tin, terbium, thorium, titanium, thallium, thulium, uranium, vanadium, yttrium, ytterbium, zinc and zirconium. The R/S ratios were most clearly related to the ionic potential of the cationic elements studied, which accounted for approximately 60% of the variability in R/S among elements. The ionic charge of an element was more important than the ionic radius. Elements with high ionic charge had low R/S ratios and vice versa. No clear differences in R/S between essential and non-essential plant nutrients were observed, especially when ions of similar charge were compared.
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PMID:Ionic charge, radius, and potential control root/soil concentration ratios of fifty cationic elements in the organic horizon of a beech (Fagus sylvatica) forest podzol. 1526 69


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