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A new on-line flow injection (FI) pre-treatment system using a disk-type chelating resin (5 mm diameter, 0.5 mm thickness) was developed for the simultaneous multi-element determination of trace metals in sea-water samples by inductively coupled plasma mass spectrometry (ICP-MS). A chelating resin possessing an iminodiacetate (IDA) functional group was used for the collection of trace elements and the elimination of alkali and alkaline earth metals in highly concentrated salt solution. A 1 ml volume of a sea-water sample (pH 5.5) was applied to the chelating resin disk. Considering the removal efficiency for Ca, 50 mM ammonium acetate buffer solution (pH 5.5) was chosen as a sample carrier. The enriched trace metals were eluted with 0.1 M nitric acid and the eluate flowed into the ICP-MS system. The processing time for one sample was < 6 min (350 s). One of the important observations is the possibility of working with a low recovery, even lower than 50%. For example, several elements such as Mn, Cr, As, Mo, Ba and U, the recovery of which was < 50% in a batch-wise method, showed good linearity and reproducibility. The proposed method was evaluated by analyzing two kinds of sea-water certified reference materials, CASS-4 and NASS-5. Analytical data for eight heavy metals, V, Mn, Co, Ni, Cu, Mo, Cd and U, obtained from the present study agreed well with the certified values.
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PMID:Inductively coupled plasma mass spectrometric determination of heavy metals in sea-water samples after pre-treatment with a chelating resin disk by an on-line flow injection method. 1214 9

A new system has been developed for the determination of total organic carbon (TOC) and inorganic carbon (IC) or total inorganic carbon (TIC) in waters. Only nonvolatile organic compounds can be detected through the present method. The system presented in this work is based on the measurement of the carbon atomic emission intensity in inductively coupled plasma atomic emission spectrometry (ICP-AES). This way, the organic matter does not undergo any preoxidation step. A semiautomatic accessory connected to the spectrometer separates the different carbon fractions (i.e., organic and inorganic). Because most of the solutions used in the present work did not contain suspended solid particles, the actual parameter that was determined was the dissolved organic carbon (DOC). The present system exhibits good sensitivities compared to those provided by conventional TOC and IC determination methods. The limits of detection obtained in the present work have been 0.07 and 0.0007 mg/L C in terms of TOC and IC, respectively. Furthermore, the system is able to handle high-salt-content solutions. This fact suggests that it would be possible to analyze seawater samples, avoiding some of the problems encountered with conventional methods, such as system blocking or interferences. The TOC and IC values found for natural samples are very close to those measured using conventional methods. The ICP-AES method has been successfully used in two interesting applications: (i) monitoring the efficiency of a water treatment plant and (ii) determining the contents of dissolved carbon dioxide, on one hand, and that of carbonate and bicarbonate, on the other, in the same sample.
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PMID:A system for the direct determination of the nonvolatile organic carbon, dissolved organic carbon, and inorganic carbon in water samples through inductively coupled plasma atomic emission spectrometry. 1253 Aug 26

A previously developed microwave heated vapor-phase digestion method for biological samples was modified to enable digestion of difficult to digest organic samples. Organic samples containing ca. 100 mg of organic carbon were digested using volume calibrated quartz inserts inside second generation type medium pressure microwave vessels. As digestion reagents, 98% sulfuric acid, 70% nitric acid and 30% hydrogen peroxide were used. The accuracy of the method was tested with six certified reference materials. Elements Ca, Fe, K, Na, Mg, P and Zn were determined from NIST-SRM 8433 corn bran. Elements Al, Fe, Cd, Cu, and Zn were determined from NRCC DOLT-2 dogfish liver. The element Cd was determined from IRMM-VDA Cd in polyethylene No. 001-004 reference materials. These elements were determined from digested samples by ICP-OES. The results were close or within certified limits. The modified method could digest nearly all the materials tested, including the above mentioned reference materials, 2-nitrobenzoic acid (2-NBA), 4-NBA and copper(II) phthalosyanine-3, 4',4',4'-tetrasulfonic acid tetrasodium salt (CPS). The method could not digest 3-NBA.
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PMID:Development of a modified medium pressure microwave vapor-phase digestion method for difficult to digest organic samples. 1262 63

A new method for determining iodine had been developed in ICP-AES. An oxidant, NaNO2 and a sample containing iodine ion were mixed in the PHD hydroid generation device, the producing iodine molecules were nebulized in nebulizer and then the iodine gas came into troch directly. The problem that the intensity of iodine decreases with the increase of time was solved. It was found that NaNO2 decreased the effect of Cl- in the low acidity. A detection limit of 14 ng.mL-1 was obtained and the RSD of the measurement for 2 micrograms.mL-1 of iodine was 1.2% (n = 10). The average recoveries of iodine were 99.44%. The method was applied to the determination of salt and seawater.
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PMID:[Study on the determination of iodine by inductively coupled plasma atomic emission spectrometry]. 1294 71

An investigational drug (A) in its calcium salt form has been developed as the tablet dosage form. Monitoring drug distribution and uniformity in granules and tablets during early stage formulation/process development is critical for drug product quality control and process robustness. In this report, an efficient and reliable analytical method for monitoring drug compound A uniformity and distribution has been developed by analyzing calcium, the counter ion of the drug substance, by Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). In this method, calcium in compound A granule and tablet samples was digested with 1 M hydrochloric acid by heating at 90 degrees C for 2 h. The resulting suspension was centrifuged, and the supernatant was directly aspirated into an ICP-AES. This method has been validated to demonstrate satisfactory precision, accuracy, specificity and sensitivity. Finally, this method has been used to analyze sieve fraction granules and tablets of drug compound A. The data generated were highly comparable to those by validated HPLC methods (UV method can not be applicable due to significant bias). In comparison with HPLC methods, this method demonstrates a significantly improved efficiency with very short analysis time (1 min per sample), and can be used as an excellent alternative for UV and HPLC methods to support formulation screening.
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PMID:Determination of content uniformity and distribution characteristics of an investigational drug in its tablets dosage form and granule by ICP-AES. 1465 86

BACKGROUND: It is estimated that over 80% of respirable particulate matter (PM10) in cities comes from road transport and that tire and brake wear are responsible for the 3-7% emission of it. Data on the indicators of environmental impact of tire debris (TD), originated from the tire abrasion on roads, are extremely scarce, even though TD contains chemicals (zinc and organic compounds) which can be released in the environment. METHODS: TD particle morphology was analysed with SEM, TEM and FIB instruments. TD eluates and TD organic extracts were tested at dilution series on human cell lines and Xenopus laevis embryos. 50 and 100 g/L TD were used for the eluates obtained after 24 h at pH 3 and the quantity of zinc present was measured with a ICP-AES. Eluates diluted to 1%, 10%, 50% in culture media and undiluted were used on X. laevis embryos in the FETAX test. HepG2 cells were exposed for 24 h to 0.05 - 50 mug/ml of zinc salt while A549 cells were exposed for 24, 48 and 72 h to 10, 50, 60, or 75 mug/ml of TD extract. X. laevis embryos were exposed to 50, 80, 100, or 120 mug/ml TD extract. RESULTS: The solution of undiluted 50 g/L TD produced 80.2% mortality (p < 0.01) in X. laevis embryos and this toxic effect was three times greater than that produced by 100 g/L TD. Zn accumulation in HepG2 cells was evident after 4 h exposure. A549 cells exposed to TD organic extract for 72 h presented a modified morphology, a decrease in cell proliferation and an increase in DNA damage as shown by comet assay. The dose 80 mug/ml of TD extract produced 14.6% mortality in X. laevis embryos and 15.9% mortality at 120 mug/ml. Treatment with 80, 100, or 120 mug/ml TD organic extract increased from 14.8% to 37.8% malformed larvae percentages compared to 5.6% in the control. CONCLUSION: Since the amount of Zn leached from TD is related to pH, aggregation of particles and elution process, the quantity of TD present in the environment has to be taken into account. Moreover the atmospheric conditions, which may deeply influence the particle properties, have to be considered. The TD organic fraction was toxic for cells and organisms. Thus, because of its chemical components, TD may have a potential environmental impact and has to be further investigated.
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PMID:Impact of tire debris on in vitro and in vivo systems. 1581 62

Several roadside soil samples were collected at two field sites in Sweden. They were analysed for total elemental content (using both ICP-MS and XRF) and stable lead isotopes. Extraction with deicing salt solution and sequential extraction were performed in order to elucidate the potential mobility due to the use of deicing agents. The total concentrations of elements, especially lead, have decreased and lead is presently almost at background concentrations (15-51 ppm for surface samples). However, the isotopic signature indicates that old gasoline lead still is left at the site constructed prior to 1975. The field site constructed in 1992 showed, however, no 206Pb/207Pb ratio below 1.14. Only minor amounts were leached using deicing salt solutions; for lead only 0.29%, on average, was extracted indicating that the mobile fraction already was released. Sequential extraction indicated that lead mainly was associated with reducible (34.4%) and oxidisable (35.4%) fractions. Exchangable and acid soluble fractions contained 20.3% while 10.0% was found in the residual fraction. The salt extraction released, however, very low concentrations indicating that most in fraction 1 is acid soluble (e.g. carbonates). Tungsten was also found at high concentrations indicating a possible impact from studded tires. For tungsten the following composition was obtained: residual (48.0%) > oxidisable (47.6%) > reducible (3.3%) > exchangeable/acid soluble (1.1%). From the isotopic studies it was also suggested that the order for incorporating anthropogenic lead into soils is exchangeable/carbonates > (hydr)oxides > organic matter > residual. The multivariate technique principal component analysis (PCA) seems promising for evaluating large sequential extraction datasets.
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PMID:Metal leachability and anthropogenic signal in roadside soils estimated from sequential extraction and stable lead isotopes. 1588 69

Conducting polypyrrole (PPy) powder synthesized by using FeCl3 x 6 H2O and/or Fe(NO3)3 oxidants was impregnated in silver salt solutions. The stability and decomposition of the material was followed by thermogravimetric measurements. The total silver content was determined by atom absorption spectroscopy (ICP-AAS). The heat and electric conductivities of the composites were measured and correlated with the silver content. The incorporated silver was speciated and measured by X-ray diffraction (XRD). The spectra proved that the chemical state of the silver incorporated into the composite depends on the anion used in the polymerization process. In the case of the polymerization in a nitrate ion containing solution, the impregnation leads exclusively to the formation of metallic silver. The size distribution of the AgCl and Ag nanoparticles, determined from transmission electron microscopy (TEM) pictures in the different composites, proves the formation of a rather uniform species below 10 and 7 nm, respectively. The observations can be correlated with the different interactions in the PPy-chloride/nitrate-silver systems. The redox type interaction based conclusions can be considered as a guide during the preparation of other metal-conducting polymer composites.
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PMID:Characterization of polypyrrole-silver nanocomposites prepared in the presence of different dopants. 1685 34

Intrahepatic cholestasis of pregnancy (ICP) is a cholestatic disorder that usually develops in the third trimester of pregnancy and persists until delivery. The cause of ICP remains elusive, but there is evidence that mutations in the canalicular ABC transporter phospholipid flippase (MDR3) and in the bile salt export pump (BSEP) can predispose for the development of ICP. MDR3 and BSEP were investigated by gene sequencing and immunofluorescence microscopy in a patient with severe ICP of early onset. ICP was diagnosed in a patient in the first trimester of pregnancy with severe pruritus, elevated levels of bile salts, and 48-fold elevation of transaminase levels. A liver biopsy specimen showed diminished canalicular expression of the bile salt export pump BSEP, while the expression and localization of the phospholipid flippase MDR3 was normal. Gene sequencing revealed a homozygous MDR3 gene mutation (S320F). The patient was also homozygous for the common BSEP polymorphism V444A. Treatment with ursodeoxycholate normalized transaminase levels but could not prevent further elevation of bile salt levels and preterm delivery. The combined homozygous alterations of the canalicular transporters may explain the early onset and severity of ICP in this patient. The common BSEP polymorphism V444A accounts for the reduced canalicular BSEP expression. Reduced bile salt secretion through BSEP may explain the persistence of elevated bile salt levels and incomplete efficacy of ursodeoxycholate treatment.
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PMID:Combined mutations of canalicular transporter proteins cause severe intrahepatic cholestasis of pregnancy. 1689 Jun 14

A field study was carried out at six locations in the Lazio region (Central Italy) aimed at characterising atmospheric particulate matter (PM10 and PM2.5) from the point of view of the chemical composition and grain size distribution of the particles, the mixing properties of the atmosphere, the frequency and relevance of natural events. The combination of four different analytical techniques (ion chromatography, X-ray fluorescence and ICP for inorganic components, thermo-optical analysis for carbon compounds) yielded sound results in terms of characterisation of the air masses. During the first three months of the study (October-December 2004), many pollution events of natural (sea-salt or desert dust episodes) or anthropogenic nature were identified and characterised. More than 90% of the collected mass was identified by chemical analysis. The central role played by the mixing properties of the lower atmosphere when pollution events occurred was highlighted. The results show a major impact of primary anthropogenic pollutants on traffic stations and a homogeneous distribution of secondary pollutants over the regional area. An evaluation of the sources of PM and an identification of possible reliable tracers were obtained using a chemical fractionation procedure.
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PMID:Inorganic constituents of urban air pollution in the Lazio region (Central Italy). 1689 3


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