Gene/Protein Disease Symptom Drug Enzyme Compound
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A method for determining phosphine was developed using adsorption sampling followed by colorimetric measurement. Two types of adsorbent used in this study were prepared from silica gel by impregnation with potassium permanganate (1% w/w) or (mercury(II) chloride and sodium chloride) (0.2 + 0.2% w/w). Each adsorbent (150 mg) packed in a glass tube had the capacity to adsorb 0.3 ppm of phosphine in 3 l of test gas passing through at a rate of 300 ml/min without breakthrough. The adsorbed phosphine was desorbed into solutions as phosphate and the recovered phosphate was determined by ICP-AES or by one of two kinds of colorimetric methods for phosphate based on the molybdenum blue method, i.e., the colorimetric method following JIS K 0102 and that following the NIOSH Manual of analytical method, No. S 332. When 0.01 ppm of phosphine in 3 l of test gas was adsorbed on the potassium permanganate adsorbent and determined by the JIS method, 93.8% of the phosphine was recovered as phosphate with a CV of 12.9% (n = 3). This method was applicable to field surveys of phosphine in workplaces. The other method with the mercury(II) chloride adsorbent followed by the NIOSH method resulted in lower recovery of phosphate in low phosphine concentration range. ICP-AES was less sensitive than the colorimetries. The effect of coexistent arsenite or silicate on the colorimetry of phosphate was assessed.
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PMID:Determination of phosphine by adsorption sampling with modified silica gel and colorimetry of phosphate. 217 61

Treatment of sonicated calf thymus DNA with the antitumor active metallocene Cp2MoCl2 afforded a metallocene-DNA complex which was characterized by 31P NMR spectroscopy. In addition to the resonance for the phosphate backbone (delta-1.6), the spectrum contained 2 signals assigned to a phosphate bound Mo-DNA complex(es) (delta 37.2, 36.5) and a broad signal at delta 6.2 ppm. This result suggests that covalent attachment of the metallocene Cp2MoCl2 occurs via phosphate(O) coordination and is accompanied by local distortion of the DNA backbone. This result supports recent ICP studies with Cp2TiCl2 that have DNA detected DNA-metallocene adducts.
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PMID:A 31P NMR study of the interaction of the antitumor active metallocene Cp2MoCl2 with calf thymus DNA. 848 61

The Japanese serow (Capricornis crispus) is protected as a special natural monument in Japan. The ring count of the soft X-ray photographs of Japanese serow horn was found to be a useful criteria to determine the ages exactly. The mineralization process in Japanese serow horn was examined microscopic, ICP and X-ray diffraction methods. The incremental lines appeared as light and dark layers in the section stained for fuchsin and methylen blue. Mineral depositions were observed among the keratin fibers, no matrix vesicle in the electron dense regions. X-ray diffraction pattern of crystalline inorganic components in Japanese serow horn was determined as beta-tricalcium phosphate (TCP), hydroxyapatite (HA) and unknown phase. ICP measurement was also carried out. The horn contained trace elements of K besides Na, Ca, Fe and P. The Ca/P molar was found to be 2.9. The ratio was much higher than the theoretical value of HA. Presumably, keratin was the seed which might be related to mineralization and higher Ca activity was detected in the initial phase of epitaxial growth. Analytical results of the measurement of trace elements in Japanese serow horn by using ICP method seemed to be correlated with the evaluation of environmental conditions. The present study indicated that the mineralization of Japanese serow horn directly related with deposition Ca-deficient HA among the keratin fibers.
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PMID:The mineralization of crystalline inorganic components in Japanese serow horn. 886 13

Some ambiguity is still involved in the interpretation of the growth mechanism of monodispersed hematite (alpha-Fe2O3) particles in dilute FeCl3 solutions. Namely, there are two entirely different proposals on this issue, viz. aggregation of preformed primary particles of alpha-Fe2O3 itself and reprecipitation of the ionic species through dissolution of the preformed beta-FeOOH particles. In order to resolve this problem, the formation process was followed in detail through TEM, Electron Diffraction, XRD, FT-IR, and ICP spectrometry along with quantitative analyses on seed effects. As a result, it has been concluded that the nuclei of the hematite particles are initially generated with the formation of beta-FeOOH particles and that they are grown by deposition of the solute originally present in the solution phase and indirectly furnished from the beta-FeOOH by dissolution. As the concentration of the solute is lowered by the growth of the hematite particles, they continue to grow with the solute provided mainly from the beta-FeOOH in a steady-state of the dissolution of beta-FeOOH and growth of alpha-Fe2O3. The basic formation mechanism is common to the ellipsoidal particles grown in the presence of phosphate ions and spherical particles in their absence.
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PMID:Formation Mechanism of Monodispersed alpha-Fe2O3 Particles in Dilute FeCl3 Solutions 897 68

The efficiency of ruthenium complexes for photosensitizing DNA damage depends on the oxidizing character of their ligands. Here we report on the difference in behavior of tris(2.2'-bipyrazyl)ruthenium(II) (Ru[bpz]3(2+)), tris(2,2'-bipyridyl)ruthenium(II) (Ru[bipy]3(2+)) and cis-dichlorobis (2,2'-bipyrazyl)ruthenium(II) (Ru[bpz]2Cl2). Upon irradiation at 436 nm, Ru(bpz)3 (2+) was far less stable than Ru(bipy)3(2+). Ru(bpz)3(2+) in phosphate buffer containing NaCl undergoes a photoanation reaction leading to the formation of Ru(bpz)2Cl2, as previously reported also in organic media. In the presence of phage phi X174 DNA, Ru(bpz)3(2+) photosensitized the formation of single strand breaks with an efficiency that was, at the beginning of irradiation, similar to that of Ru(bipy)3(2+). After 8 min of irradiation, the cleavage efficiency of Ru(bpz)3(2+) reached a plateau that may correspond to its photode composition. For the same conditions, Ru(bpz)2Cl2 did not induce DNA breakage. Scavenging experiments showed that, in the presence of oxygen, DNA cleavage induced by Ru(bpz)3(2+) partly resulted from the formation of singlet oxygen and hydroxyl radical while in the absence of oxygen an additional mechanism involving electron transfer between the excited state of the ruthenium complex and DNA is proposed. The ICP measurement showed that Ru(bpz)3(2+) and Ru(bpz)2Cl2 gave rise to covalent binding onto DNA in contrast with Ru(bipy)3(2+), which did not bind to DNA under the experimental conditions. The results are discussed with regard to the potential use of these photosensitizers in phototherapy.
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PMID:Comparative study of Ru(bpz)3(2+) Ru(bipy)3(2+) and Ru(bpz)2Cl2 as photosensitizers of DNA cleavage and adduct formation. 911 40

An implementation of the Dionex IonPac AS12A analytical column with an element-specific ICP-MS detection is described for the simultaneous determination of halogen and oxyhalogen anions, sulfate, phosphate, selenite, selenate and arsenate. The chromatographic separation was achieved in less than 4 min with an aqueous 11 mM (NH4)2CO3 (pH 11.2, adjusted with aqueous ammonia) as eluent. Special emphasis was given to optimize the ICP-MS detection conditions for the reliable detection (RSD<5%) of bromate and bromide at a bromine concentration level of 1.0 microg l(-1) with 50 microl sample injection volume. In order to achieve the highest detector response for bromine species an ultrasonic nebulizer equipped with a membrane desolvator had to be employed. The detection limits (S/N=3, sample injection volume 50 microl) obtained with the IC-ICP-MS after the optimization were 0.67 microg l(-1) for BrO3-, 0.47 microg l(-1) for Br-, 69 microg l(-1) for ClO2-, 4 microg l(-1) for Cl-, 47 microg l(-1) for ClO3-, 13 microg l(-1) for SO4(2-), 36 microg l(-1) for PO4(3-), 0.4 microg l(-1) for SeO3(2-), 0.3 microg l(-1) for SeO4(2-), and 0.4 microg l(-1) for AsO4(3-).
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PMID:Determination of bromide, bromate and other anions with ion chromatography and an inductively coupled plasma mass spectrometer as element-specific detector. 1058 39

This in vitro study evaluated the corrosion resistance of a titanium nitride (TiN) ion-plated magnetic stainless steel (447J1) for the purpose of applying a magnetic attachment system to implant-supported prostheses made of titanium. The surface hardness of the TiN ion-plated 447J1 alloy with varying TiN thickness was determined prior to the corrosion testing, and 2 micrometers thickness was confirmed to be appropriate. Ions released from the 447J1 alloy, TiN ion-plated 447J1 alloy, and titanium into a 2% lactic acid aqueous solution and 0.1 mol/L phosphate buffered saline (PBS) were determined by means of an inductively coupled plasma atomic emission spectroscopy (ICP-AES). Long-term corrosion behaviour was evaluated using a multisweep cyclic voltammetry. The ICP-AES results revealed that the 447J1 alloy released ferric ions into both media, and that the amount of released ions increased when the alloy was coupled with titanium. Although both titanium and the TiN-plated 447J1 alloy released titanium ions into lactic acid solution, ferric and chromium ions were not released from the alloy specimen for all conditions. Cyclic voltamograms indicated that the long-term corrosion resistance of the 447J1 alloy was considerably improved by ion-plating with TiN.
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PMID:Corrosion resistance of a magnetic stainless steel ion-plated with titanium nitride. 1079 99

A method for phosphopeptide identification by capillary liquid chromatography (muLC) interfaced alternatively to element mass spectrometry (inductively coupled plasma mass spectrometry, ICPMS) and to electrospray ionization mass spectrometry (ESI-MS) is described. ICPMS is used for 31P detection and ESI-MS provides the corresponding molecular weight information. Alignment of the two separate muLC runs is performed using the baseline distortion at the elution front, which shows up in both muLC-ICPMS and muLC-ESI-MS. Both a quadrupole and a magnetic sector field mass analyzer were used in combination with ICP. The detection limit achieved for the muLC-ICP-HRMS runs is approximately 0.1 pmol of phosphopeptide injected. Without any further precautions, contamination by phosphate-containing compounds at this level was found to be uncritical. The method is demonstrated for the analysis of a complex mixture of synthetic phosphopeptides and a set of tryptic digests of three phosphoproteins. These include beta-casein, activated human MAP kinase ERK1, and protein kinase A catalytic subunit. The tryptic phosphopeptides of these proteins could all be detected and identified by our new strategy. Analysis of three fractions of protein kinase A catalytic subunit with different phosphorylation status gives direct access to the order in which the phosphorylation of the four phosphorylation sites occurs. The two most important aspects of using muLC-ICPMS with 31P detection for phosphopeptide identification are (i) that a high selectivity is achieved and (ii) that the signal intensity is independent of the chemical form of phosphorus and directly proportional to the molar amount of 31P in the muLC eluate. Thus, muLC-ICPMS with 31P detection is introduced as a new, robust, and specific method in phosphoproteomics.
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PMID:Analysis of protein phosphorylation by capillary liquid chromatography coupled to element mass spectrometry with 31P detection and to electrospray mass spectrometry. 1119 5

Analytical procedures for the determination of free and total sulfate and phosphate in glycosaminoglycans by high-performance liquid chromatography were studied. A column-switching method coupling high-performance size-exclusion chromatography (HPSEC) and ion chromatography (IC) is proposed for the determination of free anions. Good run-to-run and day-to-day precision values (RSD) of < 4.7% were obtained for both anions. Total anion contents were determined after wet acid hydrolysis with nitric acid-hydrogen peroxide (5 + 1) by single-column IC and ICP-AES elemental analysis in order to validate the results. Recoveries ranging from 94.6 to 99.0% for sulfate and from 80.8 to 94.0% for phosphate were obtained. Both HPSEC-IC and single-column IC methods were applied to the analysis of a low molecular mass heparin, a non-fractionated heparin and a chondroitin 4-sulfate. From the free and total sulfate determinations, the content of linked sulfur was calculated and ranged from 5.1 to 12.2% m/m.
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PMID:Determination of free and total sulfate and phosphate in glycosaminoglycans by column-switching high-performance size-exclusion and ion chromatography and single-column ion chromatography. 1123 98

This study describes a method for the determination of phosphorus in lyophilized Haemophilus influenzae type b conjugate vaccines by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). The concentration of polysaccharide is directly related to the concentration of phosphorus as measured in the laboratory. Phosphorus is present in the polyribosyl-ribitol phosphate (PRP) group of the Haemophilus influenzae type b conjugate vaccine. The repeating unit of PRP is 3-B-D ribose[1-1]ribitol-5-phosphate. Phosphorus in the final container is measured in microg per dose. The amount of PRP is calculated from this and reported in microg per dose. The Haemophilus influenzae type b conjugate vaccine was analyzed for phosphorus content within the range of 1.34 to 2.02 microg phosphorus per ml. The relative difference of phosphorus concentrations determined by the ICP-AES method from the phosphorus concentrations determined by the traditional colorimetric molybdate method ranged from 2.2 to 10.6%. Phosphorus spike recovery for the vaccine ranged from 93 to 99% (1.93+/-0.13 microg P/ml). The phosphorus determination of NIST SRM 3139 phosphorus spectrometric solution differed by 3.0% from the certified phosphorus value (10.00 mg P/ml).
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PMID:The determination of phosphorus in Haemophilus influenzae type b conjugate vaccines by inductively coupled plasma-atomic emission spectrometry. 1123 58


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