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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

The analysis of trace elements in biological samples will extend our understanding of the impact that environmental exposure to these elements has on human health. Measuring arsenic content in nails has proven useful in studies evaluating the chronic body burden of arsenic. In this study, we developed methodology with inductively coupled plasma-mass spectrometry (ICP-MS) for the determination of total arsenic in nails. We assessed the utility of the washing procedures for removing surface contamination. Four types of preanalysis treatments (water bath, sonication, water bath plus sonication, and control) after sample decomposition by nitric acid were compared to evaluate the digestion efficiencies. In addition, we studied the stability of the solution over 1 wk and the effect of acidity on the arsenic signal. Arsenic content in the digested solution was analyzed by using Ar-N2 plasma with Te as the internal standard. The results suggest that washing once with 1% Triton X-100 for 20 min for cleaning nail samples prior to ICP-MS analysis is satisfactory. Repeated measurement analysis of variance revealed that there was no significant difference among the various sample preparation techniques. Moreover, the measurements were reproducible within 1 wk, and acidity seemed to have no substantial influence on the arsenic signal. A limit of detection (on the basis of three times the standard deviation of the blank measurement) of 7 ng As/g toenail was achieved with this system, and arsenic recoveries from reference materials (human hair and nails) were in good agreement (95-106% recovery) with the certified/reference values of the standard reference materials. ICP-MS offers high accuracy and precision, as well as high-throughput capacity in the analysis of total arsenic in nail samples.
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PMID:Determination of total arsenic concentrations in nails by inductively coupled plasma mass spectrometry. 1007 18

Carp (Cyprinus carpio) were tested for cadmium accumulation and elimination during and after a simulated pollution exposure. Fish were distributed in two 1000-l indoor concrete aquaria supplied with a continuous flow (8 l min(-1)) of well water. The cadmium concentration was maintained at 53 microg l(-1) in one aquarium and 443 microg l(-1) in the other aquarium for 127 days. The exposure phase was followed by a 43-day depuration period. The cadmium accumulation in liver, kidney and muscle was measured by means of ICP-MS. The data showed that cadmium exposure produces significant cadmium uptake in tissues. Cadmium concentrations increased sharply in kidney and liver, whereas the pollutant level in muscle was only significant after 106 days. After 127 days of Cd exposure (53 microg l(-1)), the cadmium concentration in kidney was 4-fold higher than in liver and 50-fold higher than in muscle for a toxic level of 53 microg l(-1). At a Cd of 443 microg l(-1), kidney cadmium content was 2-fold higher than in liver and 100-fold higher than in muscle. In kidney and liver, the toxic concentration increased as the concentration of pollutant in water increased. During the 43 depuration days, the loss of accumulated cadmium was rapid and immediate in muscle. Conversely, no loss of cadmium was observed in kidney and liver.
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PMID:Kinetics of cadmium accumulation and elimination in carp Cyprinus carpio tissues. 1033 95

Quadrupole Inductively coupled plasma mass spectrometric (QICP-MS) and electrothermal atomic absorption spectrophotometric (ETAAS) methods for the determination of Pb and Cd in whole blood and Al, Cd, Co and Ni in urine were compared. Simple sample pretreatments were used for both instrumental techniques. Urine samples were diluted with either Millipore water or dilute HNO3, while blood samples were diluted with a solution containing either 0.14M NH3 or 0.03 M NH3, 0.05% EDTA and 0.05% Triton X-100 in Millipore water. Scandium, yttrium and indium were used as internal standards for ICP-MS measurements and (NH4)2HPO4 as a chemical modifier for the determination of Pb and Cd by ETAAS. For ICP-MS analysis, pneumatic nebulization was used for introduction of urine samples and flow injection for introduction of blood samples. Matrix matched standards were used for all calibrations and methods were validated by analyzing reference materials and samples from external quality assurance programmes. Concentrations of the listed metals were determined in blood and urine samples obtained from a healthy non occupationally exposed population and reference samples, using both instrumental techniques. The study group (n = 90) was randomly selected from a study population (n = 220) recruited from three regions considered representative of the environment encountered by the majority of the United Kingdom population. Males and females were equally represented and ranged in age from 17-65 yrs. The correlation between results obtained by the two techniques was good for all elements measured, ranging from r = 0.88 for Co in urine to r = 0.99 for both Pb and Cd in blood.
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PMID:A comparison of inductively coupled plasma mass spectrometry with electrothermal atomic absorption spectrophotometry for the determination of trace elements in blood and urine from non occupationally exposed populations. 1044 25

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

Metal concentrations have been measured in water and sediments of the Jose Antonio Alzate Reservoir, Mexico, using EDXRF and ICP techniques. Spatial and temporal distributions of total metal levels have been identified; no organised pattern was detected for any particular metal concentration. Temporal variations of metal concentrations show evidence of the water self-cleaning capacity of the reservoir, despite the high-level metal contamination determined.
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PMID:Heavy metal concentrations in water and bottom sediments of a Mexican reservoir. 1050 57

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

Fifty-six bottled mineral waters bought at random all over Europe were analysed for 66 chemical elements by ICP-AES, ICP-MS and IC-techniques. Results show that there is a wide spread in the chemical composition of mineral waters. The EEC drinking water safeguard values for chemical constituents do not apply to mineral water, although mineral water is increasingly used for general drinking water purposes. Only 15 of the randomly selected 56 mineral waters would fulfil the drinking water regulations for all parameters where action levels are defined. Differences in chemical composition observed between countries or regions are due to geological environment and to different taste or local regulations of what is mineral water. There are indications that element concentrations for some unwanted constituents (e.g. Pb) are higher in waters sold in glass bottles than in those in plastic bottles. Some elements show a clear regional dependency. Studying the large natural variation in concentration for many of the 66 studied elements it becomes clear that we know little about the natural variation of element concentration in water and the health effects of most elements in drinking water.
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PMID:Variation of 66 elements in European bottled mineral waters. 1063 88

Concentrations of 22 elements were determined in blubber, liver, kidney and muscle of five male and five female, 8-month-old harp seals (Phoca groenlandica) by ICP-MS. Young harp seals are hunted during the spring and fall and represent an important traditional dietary item for some northern fishing communities. Interest in the commercial use of seal meat products and the limited data on the level of contaminants in tissues of harp seal beaters motivated our investigation. For most elements, concentrations in liver or kidney were greater than those in muscle. Blubber concentrations were generally lowest, but concentrations of Li, As, Sr, Ba and Pb were highest in blubber. Largest concentration factors [(tissue)/(water) > 10,000] were seen for P, Fe, Zn, Cu, Cd, Se, Mn, Ag, Pb and Co, a list that includes essential elements such as Fe and Zn, as well as several important contaminants such as Cd and Pb. Differences in concentration between male and female seals were only seen in eight of 88 element/tissue comparisons. Any effects of environmental exposure due to location or dietary intake are difficult to detect. Principle component analysis shows an association of Ca with Sr and P with S; and also a distinct grouping of the elements V, Mo, Cu and Ag.
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PMID:Essential elements and priority contaminants in liver, kidney, muscle and blubber of harp seal beaters. 1063 96

Increasing speciation demands in clinical chemistry, toxicology and nutrition have made the determination of the total elements in a sample inadequate; the amount of an element and the chemical forms in which it is present need to be known. Inductively coupled plasma mass spectrometry (ICP-MS) was used after high-performance liquid chromatographic (HPLC) separation, as was electrospray ionization mass spectrometry (ESI-MS). The effect of variation of the number of carbon atoms in perfluorinated carboxylic acids used as ion-pairing agents for the separation of selenium compounds was examined. Trifluoroacetic acid (0.1%), pentafluoropropanoic acid (0.1%) or heptafluorobutanoic acid (0.1%; HFBA) were alternatively used as additives to methanol-water (1:99, v/v) solutions as mobile phases. Reversed-phase HPLC-ICP-MS with 0.1% HFBA in the mobile phase allowed more than 20 selenium compounds to be separated in 70 min in an isocratic elution mode; the separation of natural selenium-enriched sample extracts was examined and explained. The pH of the 0.1% HFBA solution was modified with hydrochloric acid or ammonia and the pH of the sample extracts before injection was modified in order to overcome unwanted double peak formation in the chromatograms of sample extracts. Oxidations of standard gamma-glutamyl-Se-methylselenocysteine and Se-methylselenocysteine were carried out using 30% H2O2 solution and identifications of selenium-containing oxidation products were made using HPLC-ICP-MS and HPLC-ESI-MS. The principal organic oxidation product in both cases was methaneseleninic acid (MeSeO2H).
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PMID:High-performance liquid chromatography of selenium compounds utilizing perfluorinated carboxylic acid ion-pairing agents and inductively coupled plasma and electrospray ionization mass spectrometric detection. 1068 Oct 9


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