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In this work, mercury speciation in phosphorus powder matrices and soda lime glass waste from new and spent fluorescent lamp wastes has been studied by thermo-desorption/atomic absorption spectrometry (TDAAS), X-ray diffraction (XRD), cold vapor-atomic absorption (CV-AAS) and atomic emission spectrometry/inductively coupled plasma (ICP/AES). TDAAS results show the presence of oxidized forms of mercury, i.e., Hg(1+) and Hg(2+), especially in wastes with high mercury concentration. Such forms are mobile, and therefore represent a potential hazard waste material. Glass TD profiles of spent fluorescent lamps suggested the presence of mercury strongly linked to the matrix, which desorbs only at high temperatures.
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PMID:Mercury speciation in fluorescent lamps by thermal release analysis. 1461 22

The purpose of this in vitro study was to evaluate the mineral contents of root-canal dentin before and after treatment with two commonly used gutta-percha solvents: chloroform and halothane. Twenty extracted human premolars, whose crowns and apical thirds had been removed, were used. Pulp tissues were removed and the teeth were randomly divided into two groups including 10 teeth each. Root canals were enlarged with Gates Glidden burs (#1, 2, and 3). Dentin chips were obtained and saved in plates to serve as a control. Root-canal-dentin walls were then treated with chloroform or halothane for 15 min. Dentin chips were again obtained using Gates Glidden burs (#4, 5, and 6). The levels of five elements, calcium, phosphorus, magnesium, potassium, and sulfur, in each specimen were analyzed using ICP-AES (inductively coupled plasma atomic emission spectrometry) technique. Changes in the levels of the chemical elements were recorded. Differences between the groups were statistically analyzed using Mann-Whitney U test. There was a significant decrease in Ca level and significant increase in Mg level after treatment with halothane (p < 0.05). There was a significant increase in Mg level after treatment with chloroform. The changes in other elements levels after treatment with gutta-percha solvents were minimal and statistically not significant (p > 0.05). As a result it was concluded that gutta-percha solvents have effect on mineral contents of root dentin.
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PMID:Effect of gutta-percha solvents on mineral contents of human root dentin using ICP-AES technique. 1476 Sep 10

A method for the determination of trace impurities of phosphorus and arsenic in trichlorosilane with prior separation followed by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) has been developed. The preconcentration of the analytes from the sample matrix was made by adding cuprous chloride to a 10 mL trichlorosilane sample for the formation of non-volatile compounds with the elements of interest. Upon evaporation of trichlorosilane, the analytes retained in the residue were then determined in the presence of copper as modifier by ETV-ICP-MS. The dual role of cuprous chloride both in the preconcentration and instrumental determination was investigated and discussed. By meticulous control of experimental conditions, limits of detection for these two elements as low as sub-ng/g can be achieved. The method was applied to the determination of phosphorus and arsenic in a commercially available trichlorosilane sample.
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PMID:Determination of phosphorus and arsenic in trichlorosilane by electrothermal vaporization-inductively coupled plasma mass spectrometry with prior concentration by cuprous chloride. 1504 33

Analysis of Acer pseudoplatanus L. (sycamore) tree rings using ICP-MS was used to assess the impact of metal deposition on trees growing in the vicinity of a metal refinery at Prescot, north-west England compared to a reference site at Croxteth 6 km distant receiving minimal deposition. No difference in tree growth between sites was recorded. Large reductions in Cu and Cd deposition since the late 1970s was accompanied by a steep decline in Cd concentrations in the outer rings in trees close to the refinery. A similar reduction in Cu concentrations was less apparent due to a tendency for Cu to increase in the outer rings. Zinc and Ni were higher in xylem at Prescot compared to Croxteth. There was no trend in Zn concentrations at either site although Ni concentrations increased in trees close to the refinery after 1982. Manganese concentrations in xylem were much higher at Prescot; Mn levels declined until the late 1970s and then increased slightly in later years interspersed by large concentration peaks within individual years during the 1980s. There was little change in Mn concentrations in trees at Croxteth during this period. Calcium, Mg and Sr concentrations remained steady or declined slightly in rings formed since 1965 in trees at Croxteth. Concentrations of Ca, Mg and Sr were higher in rings formed prior to the mid 1970s in trees at Prescot, but declined steadily after this period, although peaks in concentrations of each element were recorded in individual years during the 1980s. Phosphorous concentrations in rings increased towards the cambium at Croxteth, although P levels decreased in rings formed after 1982 at Prescot. No difference in K concentrations between sites was recorded. Lead concentrations in xylem at both sites declined steadily in rings formed after 1970, although concentrations were higher at the reference site. Analysis of individual sycamore tree rings appears to record short-term changes in pollution episodes, with little lateral movement of elements occurring. It is suggested that changes in element concentrations in trees close to the refinery are a result of reduced metal deposition combined with increased soil acidity due to reduced buffering capacity of metal ions in rainfall.
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PMID:Analysis of tree rings using inductively coupled plasma mass spectrometry to record fluctuations in a metal pollution episode. 1509 73

An ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP-MS) was introduced in the analysis of bisphosphonates. Two compounds (alendronic acid and etidronic acid) were separated on a Dionex AS-7 anion-exchange column with dilute nitric acid employed as the mobile phase. The analytes were detected at m/z 31, as they contain phosphorus. The detection limits achieved were 0.20 mg l(-1) for alendronic acid and 0.05 mg l(-1) for etidronic acid. Since the determination of phosphorus by ICP-MS is difficult due to polyatomic interferences at m/z 31 (15N16O+, 14N16O1H+, and 12C1H(3)16O+), a detailed study of the influence of plasma parameters on phosphorus and background signal was performed.
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PMID:Determination of bisphosphonates by ion chromatography-inductively coupled plasma mass spectrometry. 1525 Apr 6

Cylindrical specimens of experimental lactic acid-glass cements (6mm high x 4mm diameter) were prepared, matured at 37 degrees C for one week sealed in their molds, then exposed either to water (pH 6.6) or aqueous lactic acid (pH 2.7) for a further week. Solutions were analyzed by ICP-OES and their pH values recorded. In both solutions, cement specimens were found to release aluminum together with smaller amounts of calcium, sodium, silicon and phosphorus. They also formed soft gels that ICP-OES analysis showed were comprised mainly of aluminum and phosphorus species. These dissolution and gelation processes were accompanied by changes in the pH of the storage media (water to pH 4.9; lactic acid to 4.2). It is concluded that further work is necessary in order to fully characterize the species of aluminum released from these cements.
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PMID:The interaction of lactic acid-glass cements with aqueous solutions. 1533 49

We demonstrated that the photopatterned single-layer adsorption film of poly(1-dodecyl-4-pyridinium bromide) on a silica surface was available for a template of nickel-phosphorus (Ni-P) electroless plating through sensitization with a SnCl(2) aqueous solution and activation with a PdCl(2) aqueous solution. Four kinds of poly(1-alkyl-4-vinylpyridinium halide)s bearing methyl, propyl, hexyl, and dodecyl groups were prepared. The cationic polymers were adsorbed by a negatively charged silica surface from their solutions, to form single-layer adsorption films exhibiting desorption-resistance toward deionized water and ethanol. The organic adsorption films could be decomposed completely by exposure to 172 nm deep-UV light. The formation and decomposition of the single-layer films were confirmed by deep-UV absorption spectral measurement and zeta-potential measurement. Ni-P electroless plating was carried out on the photopatterned adsorption films, using three types of SnO(x) colloidal materials without and with cationic or anionic surfactant as catalyst precursors in the sensitization step. In the case of the negatively charged SnO(x) colloids surrounded by anionic surfactant, Ni-deposition took place preferentially on the cationic adsorption films remaining in unexposed regions. The Ni-deposition was accelerated significantly on the cationic adsorption film bearing dodecyl groups. It was obvious by ICP-AES analyses that the hydrophobic long-chain dodecyl groups in the adsorption film could promote the adsorption of the negative SnO(x) colloids on the film surface, followed by much nucleus formation of zerovalent Pd catalysts useful for the electroless plating. The result of our experiment clearly showed that, in addition to electrostatic interaction, van der Waals interaction generating between the hydrophobic long-chain hydrocarbons of the adsorption film and the surfactant improved significantly the adsorption stability of the SnO(x) colloids, resulting in highly selective Ni-deposition in accord with the photopattern shape of the cationic single-layer adsorption film.
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PMID:Selective Ni-P electroless plating on photopatterned cationic adsorption films influenced by alkyl chain lengths of polyelectrolyte adsorbates and additive surfactants. 1549 Dec 23

A comparison of different nebulisers for direct hyphenation of capillary and nano liquid chromatography (Cap-LC, Nano-LC) and quadrupole-based collision cell inductively coupled plasma mass spectrometry (CC-ICP-MS) for phosphorylation profiling of tryptic protein digests is described. Helium was used as cell gas and specially tuned instrumental conditions were used to achieve background minimisation at the mass of phosphorus, because of kinetic energy discrimination of the interfering polyatomic ions. The proposed set-up is based on a modified capillary electrophoresis interface and a home-made 4 mL spray chamber. It enables the use of gradient conditions with a highly concentrated organic mobile phase as often used in protein phosphorylation analysis, without the need to apply membrane desolvation for removal of the organic phase or further background minimisation. No significant signal suppression or other negative effects caused by the organic mobile phase occur, because of the low flow rates used in Cap-LC and the robust plasma conditions of the CC-ICP-MS instrument. A tryptic digest of beta-casein was investigated as model compound to demonstrate the applicability of the proposed set-up for phosphorylation profiling in protein analysis using quadrupole based collision-cell ICP-MS as phosphorus-specific detector. Detection limits for phosphorylated peptides down to the sub picomole level were obtained. As a complementary technique, electrospray ionisation tandem mass spectrometry (ESI-MS-MS) with data base searching was used for further characterisation of the phosphorylated peptides detected.
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PMID:Development and characterisation of a new interface for coupling capillary LC with collision-cell ICP-MS and its application for phosphorylation profiling of tryptic protein digests. 1559 18

DNA is a universal analyte found in almost every organism. It is the code that dictates our genetic make-up and it provides a vast library of information. DNA sequences can indicate genetic modification of foodstuffs, how we may metabolise pharmaceuticals and the likelihood of suffering particular diseases. The basis for many of these genetic tests would benefit greatly from procedures that can accurately quantitate DNA in an absolute manner. This would then provide a sound and universally consistent foundation for regulatory and diagnostic decision making. This work compares two different enzymatic digestion systems as precursor steps to high accuracy isotope dilution mass spectrometry (IDMS) quantitation of a 20mer oligonucleotide. In the first approach, snake venom phosphodiesterase (SVP) digests the oligonucleotide to its constituent deoxynucleotides (dNMPs), followed by liquid chromatography-IDMS (LC-IDMS) quantitation. The second enzyme digestion approach used a combination of snake venom phosphodiesterase and shrimp alkaline phosphatase (SAP) which reduces the oligonucleotide to its constituent deoxynucleosides (dNs). This was then followed by an alternative LC separation and equivalent IDMS measurements. Total phosphorous content of the 20mer oligonucleotide was measured by inductively coupled plasma optical emission spectroscopy (ICP-OES). This provided independent data for comparison with the two enzyme digestion-IDMS based procedures. The most appropriate method of quantitation was found to be the combined SVP and SAP digestion. This approach negates the need to consider and/or account for the lack of a 5' terminal phosphate residue. It also enables the use of positive ion mass spectrometry which simplifies the chromatographic requirements. Based on the exact matched IDMS of the adenine deoxynucleoside, the concentration of the original 20mer oligonucleotide was found to be 110+/-9 microg g(-1). This showed good agreement with the ICP-OES data based on the measurement of phosphorus which gave an equivalent value for the original 20mer oligonucleotide of 108+/-5microg g(-1) (uncertainties at the 95% confidence interval). It is intended that this high accuracy methodology should be used to produce high calibre reference standards. These, in turn, could then be used to underpin the quality and consistency of routine measurements involving a variety of more commonly encountered methodologies. It should be noted that the IDMS procedures are equally applicable to both sequenced and non-sequenced oligonucleotide materials.
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PMID:A comparison of enzymatic digestion for the quantitation of an oligonucleotide by liquid chromatography-isotope dilution mass spectrometry. 1568 82

The aim of this in vitro study was to evaluate mineral content of root canal dentin after treatment with several endodontic irrigation solutions. Sixty mandibular anterior teeth extracted for periodontal reasons used. The crowns of the teeth were removed at the cemento-enamel junction. Pulp tissues were removed and the teeth were randomly divided into six groups including 10 teeth each. Root canals were enlarged with gates-glidden burs (# 1, 2, and 3). The groups were treated as follows: group 1, 0.2% chlorhexidine gluconate for 15 min; group 2, 3% H2O2 for 15 min; group 3, 17% EDTA for 15 min; group 4, 5.25% NaOCl for 15 min; group 5, 2.5% NaOCl for 15 min; and group 6, distilled water (control). Dentin chips were obtained using gates-glidden burs (# 4, 5, and 6). The levels of five elements calcium, phosphorus, magnesium, potassium, and sulfur in each specimens were analyzed using ICP-AES (Inductively Coupled Plasma Atomic Emission Spectrometry) technique. Changes in the levels of the chemical elements were recorded. The results were then statistically analyzed by one-way ANOVA and Tukey tests. There was a significant decrease in the calcium and phosphorus levels after treatment with all irrigation solutions except for 5.25% NaOCl when compared with the control group (p < 0.05). The K, Mg, and S level changes were not statistically significant (p > 0.05). It has been concluded that endodontic irrigation solutions have an effect on mineral contents of root dentin.
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PMID:Effects of endodontic irrigation solutions on mineral content of root canal dentin using ICP-AES technique. 1573 66


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