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Methods are presented for the determination by ICP-MS of antimony in body fluids and tissues of infants. Urine, serum and whole blood specimens are prepared for analysis by simply diluting 200 microliters sample volumes (1 + 14) with water and adding indium as internal standard. Liver and lung tissues are digested using 16 M HNO3 either in open quartz vessels at 150 degrees C or in sealed vessels with microwave heating. The acid digests are diluted with water and indium is added as internal standard for ICP-MS measurements. All analyses were subjected to stringent internal quality control protocols. Accuracy was assessed by recoveries, repeated analyses and by analysis of NIST SRMs 1577a Bovine Liver and 1566a Oyster Tissue. Precisions of analyses were better than 5-10% in the ranges 0.1-0.3 microgram l-1 for urine, serum and blood; and at 7-25 ng g-1 in tissues. Detection limits were 0.7 ng g-1 in liver, 0.8 ng g-1 in lung, and 0.01 microgram l-1 in urine, serum and blood. The need to employ validated procedures for specimen collection and to give considerable attention to pre-analytical factors in order to avoid adventitious contamination with antimony is demonstrated.
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PMID:Determination of antimony in urine, blood and serum and in liver and lung tissues of infants by inductively coupled plasma mass spectrometry. 947 13

Electrothermal vaporization isotope dilution inductively coupled plasma mass spectrometry (ETV-ID-ICP-MS) was applied to the determination of Cd and Pb in urine samples. The isotope ratios for each element in each analytical run were calculated from the peak areas of each isotope. A relatively low vaporization temperature was used, which separated the analyte from the major matrix components and improved the ion signals of Cd and Pb significantly. Various chemical modifiers were tested to obtain the best signal of Cd and Pb. After preliminary studies, 1% HNO3 was added to the samples as the chemical modifier. The ETV-ID-ICP-MS method was applied to the determination of Cd and Pb in freeze-dried urine reference material NIST SRM 2670 and several fresh urine samples. The results for NIST SRM 2670 agreed satisfactorily with the certified values. The results for other samples obtained by isotope dilution and the method of standard additions agreed satisfactorily. The detection limits were 0.02 and 0.005 ng ml-1 for Cd and Pb, respectively. The precision between sample replicates was better than 11% for all determinations.
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PMID:Determination of cadmium and lead in urine by electrothermal vaporization isotope dilution inductively coupled plasma mass spectrometry. 983 Jan 67

All the lanthanide elements (REE) in fern (Matteuccia) and in soil were determined with inductively coupled plasma mass spectrometer (ICP-MS) in order to discuss REE behavior in fern. The fern sample was divided into three parts: root, stem, and leaf; the soil of the same site was also sampled and the soil sample was divided into two parts: HCl and HNO3 soluble part (soil[HCl]) and HF soluble part (soil[HF]). REE in each part was determined by ICP-MS after solvent extraction separation. The overall variation of the REE pattern of the root does not resemble that of the whole soil, but that of the HF soluble part. A tetrad effect variation (W-type) was found in the REE patterns of root, stem and leaf; more conspicuous tetrad effect variation was observed in HREE region than in LREE region, and was so in stem and leaf than in root. Negative anomalies of Ce were observed in the REE patterns of root, stem and leaf, with bigger anomalies in stem and leaf than in root. The results of this study suggest that REE in fern has come from silicates of soil and has once been in dissolved state.
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PMID:Distribution pattern of rare earth elements in fern: implication for intake of fresh silicate particles by plants. 984 59

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

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

The determination of all rare earth elements (REEs) in human blood serum by inductively coupled plasma mass spectrometry (ICP-MS) was performed with the aid of chelating resin (Chelex 100) preconcentration after acid digestion with HNO3 and HClO4. When chelating resin preconcentration was carried out at room temperature, the recoveries of heavy REEs were lower than those of light REEs because of their stable complex formation with residual organic compounds remaining in the digested serum solution. These problems were overcome by heating the solution at 80 degrees C during the chelating resin preconcentration process. As a result, the recoveries for all REEs were improved to 92-102% in the case of a concentration factor of 4, where the analytical detection limits for REEs were below 0.2 x 10(-12) g ml-1. Consequently, all REEs in individual human blood sera collected from five healthy volunteers could be determined by ICP-MS with good precision. The concentrations of REEs in human blood serum were extremely low, in the range from ca. 1 x 10(-12) g ml-1 of Eu to ca. 230 x 10(-12) g ml-1 of Ce.
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PMID:Determination of rare earth elements in human blood serum by inductively coupled plasma mass spectrometry after chelating resin preconcentration. 1088 74

A method for the speciation of zinc and copper binding with proteins in human serum was explored by chelating resin (Chelex-100) pre-treatment and inductively coupled plasma mass spectrometry (ICP-MS). It was shown by a SEC (size-exclusion chromatography)-ICP-MS system that albumin-zinc and albumin-copper (loosely-bound species) could be selectively removed from serum by adsorption on the Chelex-100 resin after the chelating resin pre-treatment, while alpha 2-macroglobulin-zinc and ceruloplasmin-copper (firmly-bound species) remained in the serum. The zinc and copper bound with alpha 2-macroglobulin and ceruloplasmin, respectively, were then determined by ICP-MS after batch treatment of the serum samples with the Chelex-100 resin. In addition, the total concentrations of zinc and copper were also determined by ICP-MS after a 20-fold dilution with 0.1 M HNO3. The albumin-zinc and -copper were estimated as the differences between the concentrations of total and firmly-bound species. The present batch pre-treatment method was applied to the speciation analysis of zinc and copper binding with proteins in sera donated from 25 healthy volunteers as well as from a pregnant woman and a myelodysplastic syndrome patient. The observed concentrations of alpha 2-macroglobulin-zinc and ceruloplasmin-copper were in the ranges 109-202 ng ml-1 (12.4-31.3% of total zinc) and 513-880 ng ml-1 (90.6-99.7% of total copper), respectively. The present method is simple (only addition of the chelating resin and centrifugation is required) and reproducible (average RSD = 2% for alpha 2-macroglobulin-zinc and 1% for ceruloplasmin-copper in intra-assay measurements, and 5% for alpha 2-macroglobulin-zinc and 4% for ceruloplasmin-copper in inter-assay measurements), and there is less risk of contamination during separation.
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PMID:Speciation of protein-binding zinc and copper in human blood serum by chelating resin pre-treatment and inductively coupled plasma mass spectrometry. 1088 75

A microwave digestion method in a closed vessel was developed for the determination of trace metals in atmospheric aerosols using inductively coupled plasma mass spectrometry (ICP-MS). A recovery study for the elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Sb, and Pb was conducted using multi-elemental standard solutions, NIST 1633b Trace Elements in Coal Fly Ash, and NIST 1648 Urban Particulate Matter. A simple digestion method using only HNO3/H2O2 gave good recoveries (90%-108%) for all elements except Cr in SRM 1648, but yielded low recoveries for SRM 1633b. A more robust method using HNO3/H2O2/HF/H3BO3 yielded higher recoveries (82%-103%) for the lighter elements (V-Zn) in SRM 1633b, and improved the Cr recovery in SRM 1648, but decreased the Se recovery in both SRMs. A comparative analysis of aerosol samples obtained at a remote mountain location Nathiagali, Pakistan (2.5 km above mean sea level), and Mayville, New York, downwind from the highly industrialized Midwestern United States, was carried out using Instrumental Neutron Activation Analysis (INAA) for the elements Cr, Mn, Fe, Co, Zn, As, Se, and Sb. The simple digestion method yielded excellent agreement for Cr, Fe, Zn, As, Se, and Sb, with slopes of the ICP-MS vs. INAA regressions of 0.90-1.00 and R2 values of 0.96-1.00. The regressions for Mn and Co had slopes of 0.82 and 0.84 with R2 values of 0.83 and 0.82, respectively. Addition of HF/H3BO3 did not improve the correlation for any of the elements and degraded the precision somewhat. The technique provides sensitivity and accuracy for trace elements in relatively small aerosol samples used in atmospheric chemistry studies related to SO2 oxidation in cloud droplets. The ability to determine concentrations of a very large number of elements from a single analysis will permit source apportionment of various trace pollutants and hence strategies to control the sources of air pollution. This is particularly important as the health effects of particulate matter are increasingly recognized.
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PMID:Microwave assisted digestion of atmospheric aerosol samples followed by inductively coupled plasma mass spectrometry determination of trace elements. 1121 Feb 33

An inductively coupled plasma isotope dilution mass spectrometric (ICP-IDMS) method was developed as a suitable method - with respect to its sensitivity, precision, accuracy, and time-consumption - for the analysis of toxic heavy metal traces (Pb, Cd, Cr, and Hg) in polyolefins. Results for Pb, Cd, and Cr were compared with those obtained by thermal ionization isotope dilution mass spectrometry (TI-IDMS), which was used as a reference method. Because of its high first ionization potential and its high volatility mercury could not be determined by TI-IDMS. A multi-element spike solution, containing isotopically enriched 206Pb, 116Cd, 53Cr, and 201Hg, was used for the isotope dilution step. Decomposition of the polyolefin samples was carried out with concentrated HNO3 at temperatures of about 300 degrees C in a high pressure asher (HPA). This procedure decomposes polyolefins completely and allows isotopic equilibration between sample and spike isotopes. Detection limits of 16 ng/g, 5 ng/g, 164 ng/g, and 9 ng/g were obtained for Pb, Cd, Cr, and Hg by ICP-IDMS using only sample weights of 0.25 g. In different commercially available polyethylene samples heavy metal concentrations in the range of < 5 ng/g to 4 x 10(3) ng/g were analyzed. Both mass spectrometric methods were applied within the EU project "Polymeric Elemental Reference Material (PERM)" for the certification of two polyethylene reference materials. The ICP-IDMS results agreed very well with those of TI-IDMS which demonstrates the accuracy of the ICP-IDMS method also suitable for routine analyses.
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PMID:Development of an ICP-IDMS method for accurate routine analyses of toxic heavy metals in polyolefins and comparison with results by TI-IDMS. 1122 Aug 22

For the major component analysis of Mo-Si (-B) alloys by ICP-AES, an appropriate dissolution method is necessary. The general procedure using a HNO3-HF mixture cannot be applied for Mo-Si (-B) alloys due to Si volatilization followed by violent reaction and due to MoO2 precipitation in the preparation of a Mo standard solution from metallic Mo. Good results were obtained with a mixture of 10 mL H2SO4, 1 mL HNO3, 2 mL HF and 12 mL H2O for Mo-Si (-B) alloys. The samples were completely dissolved at room temperature without any losses. A sequential correction method is also suggested to correct several errors in ICP-AES analysis such as fluctuation in the emission intensities, spectral interferences, non-spectral interferences and blank values.
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PMID:Dissolution of molybdenum-silicon (-boron) alloys using a mixture of sulfuric, nitric and hydrofluoric acids and a sequential correction method for ICP-AES analysis. 1122 63


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