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A novel approach for determination of phytic acid in cereals has been applied in 2 traditional methods. In the first, phytic acid in a sample extract is first separated and concentrated by ion-exchange chromatography. The phytic acid concentrate is then quantitatively determined as phosphorus by inductively coupled plasma atomic emission spectrometry (ICP-AES). In the second method, extracted phytic acid is first precipitated by FeCl3 solution. The complexed iron is converted to ferric hydroxide by adding NaOH, thus releasing phytic acid as soluble sodium phytate. Phytate is then quantitatively determined as phosphorus by ICP-AES. In these methods, both the difficult acid digestion and the spectrometric determination of phosphorus found in traditional methods are eliminated by using ICP-AES. This results in a method that is simpler, faster, and more accurate than earlier procedures.
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PMID:Determination of phytic acid in cereals using ICP-AES to determine phosphorus. 202 74

Inductively coupled plasma mass spectrometry (ICP-MS) allowed 0.2-0.3% imprecision (1 sigma) in 204Pb/206Pb, 207Pb/206Pb, and 208Pb/206Pb measurements at the 20-100 ppb level, which was precise enough to detect some of the isotopic variations observed in nature. Mass discrimination could be corrected within +/- 0.5% of the true value by periodical analysis of standard reference material of known lead isotopic composition. As a separation method for lead in human bone, which contains enormous amounts of calcium and phosphorus, anion exchange of the Pb-Br complex was found to be effective. Lead isotope ratios in bone, measured by ICP-MS after separation, were consistent with those measured by thermal ionization mass spectrometry. Hair matrix did not have any influence on the accuracy and precision of the analysis; a digested sample could be directly analyzed and this offered rapid sample throughput. Preliminary data on lead isotope ratios in bone and hair from prehistoric and contemporary Japanese are presented.
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PMID:Isotope ratio analysis of lead in biological materials by inductively coupled plasma mass spectrometry. 884 88

In order to make quantitative comparison between food composition table-based estimates and instrumental measures by inductively coupled plasma atomic emission spectrometry (ICP-AES), total food duplicates were collected from 232 adult women in 10 study regions in 9 Prefectures in Japan. Daily dietary intake of 5 elements, sodium (Na), potassium (K), phosphorus (P), calcium (Ca) and iron (Fe), were estimated from the weights of food items in each duplicate by use of food composition tables. Parallel to this the intakes were measured by wet-ashing of food duplicate homogenates followed by ICP-AES analysis. Because the emission intensity of K was significantly modified by Na co-present at various concentrations, K was measured after Na concentration was reduced to the value 150 mg/L by dilution. The comparison of the two sets of the results, the estimated values and the measured values, showed that the estimated values were significantly larger than the measured values in the cases of Na, K, Ca and P (the ratio of the estimated to the measured values: 118% for Na, 115% for K, 109% for Ca; and 130% for Fe), whereas the two values essentially agreed with each other in the case of P (ratio: 93%). The differences were too large for any nutritional evaluation to be made when the method of Bland and Altman is applied. The significance of the differences in relation to nutritional evaluation of element intake is discussed.
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PMID:A comparison of the food composition table-based estimates of dietary element intake with the values obtained by inductively coupled plasma atomic emission spectrometry: an experience in a Japanese population. 902 75

The quantitative determination of nucleotides from DNA modified by styrene oxide is described using a combination of inductively coupled plasma high-resolution mass spectrometry (ICP-HRMS) and electrospray ionization mass spectrometry (ESI-MS), both interfaced to reversed-phase high-performance liquid chromatography (HPLC). LC/ICP-MS (resolution > 1500 to discriminate against 15N16O+ and 14N16OH+) was employed to determine quantitatively the content of modified nucleotides in standard solutions based on the signal of phosphorus; phosphoric acid served as an internal standard. By means of the standard addition technique the sensitivity of the LC/ESI-MS approach was subsequently determined. Since a comparison of UV, ICP and ESI-MS data suggested that in ESI-MS the ionization efficiency of the adducts is identical within the error limits, quantitative determination of all adducts is possible. For LC/ESI-MS with single ion monitoring, the detection limit for styrene oxide adducts of nucleotides was determined to be 20 pg absolute or 14 modified in 10(8) unmodified nucleotides in a 5 micrograms DNA sample, which comes close to the best methods available for the detection of chemical modifications in DNA.
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PMID:Quantitative determination of DNA adducts using liquid chromatography/electrospray ionization mass spectrometry and liquid chromatography/high-resolution inductively coupled plasma mass spectrometry. 1022 66

To elucidate the element content of newborn blood vessels, umbilical arteries and veins in human umbilical cords, which had the advantage of easy sampling, were examined by ICP-AES. Umbilical cords were removed after birth. Mothers' ages ranged from 26 to 35 yr. It was found that the content of sulfur was the highest in both umbilical arteries and veins, being higher than the content of calcium and phosphorus. With respect of the content of sulfur, calcium, and magnesium, there were significant differences between the arteries and veins.
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PMID:Element content of human umbilical artery and vein in umbilical cord. 1046 60

A new method for the determination of cyclophosphamide content of polyalkylcyanoacrylate nanoparticles was developed. The analyses were carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES) by measuring the phosphorus content in the drug. The results obtained by this non-selective technique were compared with those given by high performance liquid chromatography (HPLC) a selective procedure that permits the detection of the cyclophosphamide molecule, and its degradation products. Sensitivity and reproducibility of both procedures were also determined. The ICP-AES method was demonstrated to be valid for sensitivity, precision, accuracy and specificity. In spite of ICP method is not a suitable procedure to analyze the degradation products of cyclophosphamide, the sensitivity of ICP is higher than chromatographic technique. Nevertheless, both procedures are appropriate for the determination of cyclophosphamide-loaded nanoparticles.
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PMID:An inductively coupled plasma method for determination of cyclophosphamide loaded to polymeric systems. 1070 28

Macrofungi can accumulate some minerals, including toxic metals if present in the substrate. A periodic monitoring of these elements in mushrooms is recommended when the conditions of cultivation are altered. The aim of this work was to evaluate the mineral content of Pleurotus spp (hiratake and shimeji) and of imported (chilean and italian) dehydrated mushrooms. Fresh fruiting bodies of Pleurotus spp were obtained from cultivators and dehydrated mushrooms were bought in a market. The samples were dried, milled and digested by C1H-NO3H. The content of P, K, S, Ca, Mg, Cu, Fe, Mn, Zn, Na and B were analyzed by ICP-AES and Al, Cd, Cr, Pb, Co, Ni by ICP-OES. The results classify these mushrooms as a source of potassium and copper: Pleurotus spp are also a source of phosphorus (P < 0.05); the chilean mushrooms present high content of iron (P < 0.05). All the evaluated mushrooms were identified as a food without sodium (< 5 mg Na/100 g). So these mushrooms being a source of potassium without Na, answer the needs of hypertension and/or heart diseases patients as a food and/or like a condiment for flavor enhancement. Subsequent studies should include major sampling and the evaluation of the toxic metals, Pb and Cr, employing more accurate methods of analysis, as well as the evaluation of Hg (not analysed in this study), mainly in wild mushrooms, commercialized dehydrated.
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PMID:[Mineral composition of edible mushrooms cultivated in Brazil--Pleurotus spp and other dehydrated species]. 1104 80

A new method has been utilised for the characterisation of natural particle surface coatings. The method involves the use of sedimentation field-flow fractionation (SdFFF), radiolabelling and inductively coupled plasma-high resolution mass spectrometry (ICP-HR MS) techniques to study the effect of colloidal surface coatings on the adsorptive behaviour of orthophosphate. Colloidal river sediment and soil samples were chemically treated in an attempt to selectively remove metal hydroxyoxides and natural organic matter. The samples were then radiolabelled with 33PO4(3-) and analysed by SdFFF to determine the surface adsorption density (SAD) of orthophosphate as a function of particle size. The SdFFF unit was directly coupled to an ICP-HR MS to determine the chemical composition of the colloidal samples as a function of particle size. Element concentration/UV detector signal and element atomic molar ratios were plotted against particle size, and the trends used in the interpretation of SAD distribution (SADD) changes for the samples were studied. In general, non-constant trends in the orthophosphate SADDs were found, except for the river sediment treated with hydroxylamine hydrochloride. The results indicated that, in the soil sample studied, the Mn oxide coating was a dominant factor in determining phosphorus adsorption. This method could also be applicable to other industrial or similar samples.
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PMID:The effect of surface coatings on the association of orthophosphate with natural colloids. 1119 56

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

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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