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A novel HPLC technique has been developed for the determination of carboplatinum(II) and cisplatinum(II) which are used for chemotherapy. The compounds were separated by a HPLC column. The eluent was on-line nebulized into the nebuliser gas flow using ultrasonic nebulisation. The resulting aerosol was driven by the nebuliser gas stream through a 30-cm heating path, a 60-cm cooling path for desolvatisation and into the plasma of the ICP-MS. The detection was carried out on platinum mass 195Pt. Different RP C18 techniques were tested to obtain the best separation and detection results of the two platinum compounds. The solvent-generated anion exchanger method was selected as the method with the best handling and sensitivity. This technique allows a good separation of the two compounds within 3 min. The detection limits for carboplatinum and cisplatinum were 130 and 80 pg, respectively. The newly developed system has been applied to study the behaviour of the platinum species under different anion influences in aqueous solutions. These investigations are necessary for the future development of an extraction from environmental samples for the two compounds. In further experiments the distribution of the two platinum species, Na2Pt(II)Cl4 and the palladium species. Na2Pd(II)Cl4 between water/sediment, water/charcoal, sewage sludge/water and the distribution in the solution after iron flocculation were investigated to plan an extraction method for the platinum species from environmental matrices.
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PMID:Determination of carboplatinum and cisplatinum by interfacing HPLC with ICP-MS using ultrasonic nebulisation. 1002 13

L-Glutamate dehydrogenase (GLDH) independent of NAD(P) and oxygen was first obtained from the psychrotrophic bacterium Aeromonas sp. L101, originally isolated from the organs of salmon (Oncorhynchus keta). GLDH was purified by a series of chromatography steps on DEAE-Sepharose, Superdex 200pg, Q-Sepharose, CM-Sepharose, and Phenyl-Sepharose. The purified protein was determined to have a molecular mass of 110 kDa and a pI of 5.7. Maximum activity was obtained at 55 degrees C and pH 8.5. The activity of GLDH at 4 and 20 degrees C was 38 and 50%, respectively, of that at 50 degrees C. GLDH was coupled to cytochrome c and several redox dyes including 1-methoxy-5-methylphenazinium methylsulfate (1-Methoxy PMS), 2, 6-dichlorophenylindophenol (DCIP), 9-dimethylaminobenzo[alpha]phenoxazin-7-ium chloride (meldola's blue), 3,3'-[3,3'-dimethoxy-(1,1'-biphenyl)-4, 4'-diyl]-bis[2-(4-nitrophenyl)-5-phenyl-2H tetrazolium chloride] (nitroblue tetrazolium; NBT), and 2-(4-iodophenyl)-3-(4-nitrophenyl)-5-phenyl-2H tetrazolium (INT). The presence of NAD(P) and oxygen gave no oxidation activity to GLDH. Spectroscopic profile and ICP data indicated a b-type cytochrome containing iron.
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PMID:Purification and characterization of cold-active L-glutamate dehydrogenase independent of NAD(P) and oxygen. 1010 Dec 90

Trace metal pollutants in the surface water of the Houston Ship Channel were determined using inductively coupled plasma/mass spectrometry (ICP/MS). Metal concentrations varied according to sampling sites. Barium, cobalt, chromium, molybdenum, silver, beryllium, antimony, lead, and mercury concentrations were relatively similar throughout the channel averaging 83.25, 0.55, 6. 31, 6.66, 0.02, 0.017, 3.61, 0.68, and 0.055 microg/L, respectively. Titanium, manganese, copper, zinc, nickel, and selenium concentrations were found to be higher at stations closer to the Galveston Bay (as the water is turning from relatively fresh water to sea water) with concentration ranges of 102.5-351.7, 0.3-25, 0. 3-25, 30-280, 16-77, 6.2-26.5, and 0.0-6.2 microg/L, respectively. Aluminum was found to be much higher at the Buffalo Bayou station (341 microg/L) followed by the San Jacinto station (104 microg/L) with an average of 42 microg/L in the other two stations. Vanadium was found to be unusually high at the Washburn Tunnel station (116 microg/L) and at much lower concentrations in the other three stations, averaging 6.5 microg/L. Iron was also higher at the Buffalo Bayou station (143 microg/L) but was absent at the Lynchburg Ferries station. Arsenic was not found at the Lynchburg and San Jacinto stations. However, arsenic had similar concentrations of 1. 983 and 1.835 microg/L at Buffalo Bayou and Washburn Tunnel, respectively. Cadmium was higher at the Lynchburg Ferries station (3. 3 microg/L) and ranged from 0.3 to 0.96 microg/L in the other locations. Thallium was not found in any of the stations.
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PMID:Analysis of metal pollutants in the Houston Ship Channel by inductively coupled plasma/mass spectrometry. 1049 97

Recent spectroscopic work has suggested that only one surface species of sulfate is dominant on hematite. Sulfate is therefore a very suitable anion to test and develop adsorption models for variable charge minerals. We have studied sulfate adsorption on goethite covering a large range of sulfate concentrations, surface coverages, pH values, and electrolyte concentrations. Four different techniques were used to cover the entire range of conditions. For characterization at low sulfate concentrations, below the detection limit of sulfate with ICP-AES, we used proton-sulfate titrations at constant pH. Adsorption isotherms were studied for the intermediate sulfate concentration range. Acid-base titrations in sodium sulfate and electromobility were used for high sulfate concentrations. All the data can be modeled with one adsorbed species if it is assumed that the charge of adsorbed sulfate is spatially distributed in the interface. The charge distribution of sulfate follows directly from modeling the proton-sulfate adsorption stoichiometry since this stoichiometry is independent of the intrinsic affinity constant of sulfate. The charge distribution can be related to the structure of the surface complex by use of the Pauling bond valence concept and is in accordance with the microscopic structure found by spectroscopy. The intrinsic affinity constant follows from the other measurements. Modeling of the proton-ion stoichiometry with the commonly used 2-pK models, where adsorbed ions are treated as point charges, is possible only if at least two surface species for sulfate are used. Copyright 1999 Academic Press.
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PMID:Sulfate Adsorption on Goethite. 1050 84

An alternative method for the determination of trace levels of fluoride in drinking and sea-water samples is presented. It is based on the formation of the aluminium monofluoride complex in excess of Al3+ and separation of the two species formed (AlF2+ and Al3+) in a small (5 cm long, CG2) ion exchange guard column. The final determination is accomplished by both ICP-MS specific detection and post column derivatisation with fluorimetric detection. Fundamental studies on the formation kinetics of the complex, ion chromatographic separation and optimum aluminium concentration were carried out using spectrofluorimetric detection by post-column reaction of the species with 8-hydroxyquinoline-5-sulfonic acid in a micellar medium of cetyltrimethylammonium bromide. Fluorimetric detection showed good detection limits, but interferences from cations such as Mg2+ and Zn2+ required the use of the longer CS2 ion exchange column. Iron interfered in relatively large amounts but adding EDTA to the sample solution eliminated the interference. A similar separation methodology was applied using ICP-MS detection for the indirect determination of fluoride, by monitoring aluminium at mass 27. In this case, a detection limit of 0.1 ng ml-1 was obtained using 0.45 M HNO3 as eluent and no interference caused by high concentrations of iron was observed. The proposed method was applied to the determination of very low levels of fluoride in natural waters.
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PMID:Indirect determination of trace amounts of fluoride in natural waters by ion chromatography: a comparison of on-line post-column fluorimetry and ICP-MS detectors. 1056 42

Succimer is considered to be a safe and effective treatment for lead (Pb) poisoning, since it reduces body Pb levels without an apparent diuresis of other essential elements. However, while existing clinical data indicate that succimer does not significantly increase the excretion of non-target elements, those studies have also reported a wide range of outcomes. Therefore, we investigated whether succimer treatment measurably increased the urinary excretion of essential elements in a primate model of childhood Pb exposure. Infant rhesus monkeys (Macaca mulatta) were exposed to Pb from birth through one year of age, and presented blood Pb levels of approximately 40-50 microg/dL at the start of treatment. Subsequently, they were treated with succimer (30 mg/kg/day x 5 days followed by 20 mg/kg/day x 14 days, n = 15) or vehicle (n = 14) for 19 days. Complete urine samples were collected over the first 5 days of treatment, and were analyzed for levels of calcium (Ca), cobalt (Co), copper (Cu), iron (Fe), lead (Pb), magnesium (Mg), manganese (Mn), nickel (Ni), and zinc (Zn), using trace metal-clean techniques and magnetic sector-ICP-MS. Succimer treatment significantly (p < 0.05) reduced blood Pb levels when compared to the vehicle group over the treatment period, and concomitantly produced a significant >4-fold increase in urinary Pb excretion. Succimer treatment also significantly (p < 0.05, multivariate ANOVA) increased the urinary excretion of essential elements, but only when the cumulative total excretion over treatment days 1-5 for all elements were considered. None of these relative increases reached statistical significance for any particular element x day, although increases in Zn (day 3) excretion were only marginally non-significant (0.1 > p > 0.05). Multivariate analyses of a subset of elements (Cu, Fe, Mn, Zn) similarly indicated no significant effect of succimer treatment overall, although the urinary excretion of Mn was significantly increased on day 3 of treatment. Collectively, these data indicate that succimer does contribute to an increase in the urinary excretion of essential elements, although not significantly for any single element considered here. This may be important in Pb-exposed children, who can possess reduced trace element reserves due to nutritional deficiencies.
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PMID:Succimer and the urinary excretion of essential elements in a primate model of childhood lead exposure. 1077 30

This manuscript describes the use of Supercritical-Fluid Chromatography (SFC) with plasma spectrometric detection for the analysis of organometallics. An introduction on the principles and characteristics of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) is included, along with a discussion about requirements for coupling SFC to plasma detection and the different approaches for interfacing SFC to ICP. The last part of this review paper provides a comprehensive description of SFC-ICP applications for the analysis of organometallics containing iron, silicon, tin, chromium, arsenic, lead, mercury and antimony.
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PMID:Element selective detection for supercritical-fluid chromatography. 1086 66

Macrofungi can accumulate some minerals, including toxic metals if present in the substrate. A periodic monitoring of these elements in mushrooms is recommended when the conditions of cultivation are altered. The aim of this work was to evaluate the mineral content of Pleurotus spp (hiratake and shimeji) and of imported (chilean and italian) dehydrated mushrooms. Fresh fruiting bodies of Pleurotus spp were obtained from cultivators and dehydrated mushrooms were bought in a market. The samples were dried, milled and digested by C1H-NO3H. The content of P, K, S, Ca, Mg, Cu, Fe, Mn, Zn, Na and B were analyzed by ICP-AES and Al, Cd, Cr, Pb, Co, Ni by ICP-OES. The results classify these mushrooms as a source of potassium and copper: Pleurotus spp are also a source of phosphorus (P < 0.05); the chilean mushrooms present high content of iron (P < 0.05). All the evaluated mushrooms were identified as a food without sodium (< 5 mg Na/100 g). So these mushrooms being a source of potassium without Na, answer the needs of hypertension and/or heart diseases patients as a food and/or like a condiment for flavor enhancement. Subsequent studies should include major sampling and the evaluation of the toxic metals, Pb and Cr, employing more accurate methods of analysis, as well as the evaluation of Hg (not analysed in this study), mainly in wild mushrooms, commercialized dehydrated.
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PMID:[Mineral composition of edible mushrooms cultivated in Brazil--Pleurotus spp and other dehydrated species]. 1104 80

Magnetic sector field inductively coupled plasma-mass spectrometry (ICP-MS) was applied to the reliable determination of the 8 essential trace elements cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), manganese (Mn), nickel (Ni), selenium (Se), and vanadium (V) as well as the 7 nonessential and toxic elements silver (Ag), aluminum (Al), arsenic (As), gold (Au), platinum (Pt), scandium (Sc), and titanum (Ti) in 27 transitory and mature human milk samples and in 4 selected infant formulas. This advanced instrumentation can separate spectral overlaps from the analyte signal hampering significantly the determination of many trace elements by conventional ICP-MS. Moreover, superior detection limits in the picogram per liter range can be obtained with such magnetic sector field instruments. Therefore, this is the first study to report, the concentrations of the elements Ag, Au, Pt, Sc, Ti, and V in human milk and in infant formulas. Concentrations of Ag (median: 0.41 microg/L; range: < 0.13-42 microg/L) and Au (median: 0.29 microg/L; range 0.10-2.06 microg/L) showed large variations in human milk that might be associated with dental fillings and jewelry. Pt concentrations were very low with most of the samples below the method detection limit of 0.01 microg/L. Human milk concentrations of Co (median: 0.19 microg/L), Fe (380 microg/L), Mn (6.3 microg/L), Ni (0.79 microg/L), and Se (17 microg/L) were at the low end of the corresponding reference ranges. Concentrations of Cr (24.3 microg/L) in human milk were five times higher than the high end of the reference range. For Al (67 microg/L), As (6.7 microg/L), and V (0.18 microg/L), most of the samples had concentrations well within the reference ranges. All elemental concentrations in infant formulas (except for Cr) were approximately one order of magnitude higher than in human milk.
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PMID:Concentrations of selected trace elements in human milk and in infant formulas determined by magnetic sector field inductively coupled plasma-mass spectrometry. 1104 26

Serum transferrin (Tf) is an iron-binding glycoprotein. Aluminium in the blood is bound to the transferrin. In the present study, the chemical forms of co-existing Al and Fe bound to human serum Tf were studied by combined on-line HPLC and high-resolution ICP-MS (HPLC-HR-ICP-MS). Samples were subjected to HPLC equipped with an anion-exchange column. The levels of 27Al, 56Fe and 32S, which are interfered with by polyatomic ions such as 13C14N+, 12C15N+ and 12C14N1H+, 40Ar16O+ and 40Ca16O+, and 16O2+, respectively, when using quadrupole ICP-MS, were monitored simultaneously by HR-ICP-MS at a resolution of m/delta m = 3000. Al added to apo-Tf as Al-citrate was preferentially bound to the N-lobe site almost selectively. Al in serum from a healthy person without any in vitro Al spike was present both as AlN-Tf and AlN,FeC-Tf. The chemical states were reproduced in the apo-Tf solution supplemented with Fe (Fe/Tf ratio = 0.6) and Al (Al/Tf ratio = 1) successively. The 32S level was useful for monitoring the protein levels in the HPLC eluate. The clean-up column procedures employed reduced the detection limit for 27Al to 0.1 microgram l-1 (3SB) at the middle resolution.
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PMID:Binding patterns of co-existing aluminium and iron to human serum transferrin studied by HPLC-high resolution ICP-MS. 1119 83


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