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Neutron activation analysis (NAA) and inductively coupled plasma emission spectrometry (ICP-AES) were used to quantify the relative contents of Fe, Sc, Ce, Pa, Cr, Co, respectively the absolute contents of Cr, Zn, Mn, Fe, Mg, Al, Cu, Ti, Ca, Sr in hashish samples, seized in different countries. The samples were processed after dry ashing by means of instrumental NAA and after wet mineralization by means of ICP-AES. For determination of the sampling and measurement errors, one of the samples was analyzed repeatedly with both methods. Classifying hashish samples with regard to concentration of certain elements could be done by artificial neural networks with a modified backpropagation algorithm. By this way, identity and non identity of one unknown sample with one of many different samples as data pool can be ascertained, on principle.
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PMID:[Identification of hashish samples with inductively coupled high-frequency plasma emission spectrometry and neutron activation analysis and data handling with neuronal networks. 1. Methods for the quantitative determination of characteristic trace elements]. 944 7

An HPLC method with UV/VIS and ICP-AES detection is described for the determination of vanadyl porphyrins extracted from biological samples. A detection limit of 50 ng of vanadium was obtained. The method was used to determine these compounds following their extraction from tissues of mussels treated in laboratory experiments and collected during a 'Mussel Watch Programme'. This allowed some conclusions about vanadium speciation in marine organisms to be made. In the tissues of mussels, collected at several sites of the monitored area, which showed high vanadium concentrations, it was possible to establish the presence of this metal in the form of organometallic compounds.
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PMID:Determination of trace amounts of vanadyl porphyrin in marine mussel tissues by high-performance liquid chromatography with both ultraviolet/visible and inductively coupled plasma atomic emission spectrometric detection. 946 57

Twenty different hashish samples, which were confiscated in Irak, Iran, Bulgaria, Switzerland, Great Britain and Germany were analysed by means of NAA and ICP-AES. We used modified ANNs to identify a repeated analysed sample out of that data pool. The ANNs are described. Especially the learning rule, a modified backpropagation method, is presented. It is obvious, that neural networks can solve the described classification tasks. There is no significant difference in the power of the applied analytical methods.
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PMID:[Testing the identity of hashish samples with ICP-AES and NAA and data handling with neural networks. 2. Data verification with the use of artificial neural networks]. 947 57

PAH emission from the powered engines fueled by a 95 leadfree gasoline (95-LFG), a 92 leadfree gasoline (92-LFG) and a Premium leaded gasoline (PLG) with two gasoline additives (SA and SB) were collected using a PAH sampling system with a particulate interception device. Twenty one PAHs were analyzed primarily by an GC/MS, while eight metal elements were determined mainly by an ICP-AES. This investigation showed that the gasoline additives contain more amounts of carcinogenic PAHs than gasolines do. Blending these additives do raise the PAH content in the gasolines, simultaneously, will emit more amount of PAHs from the tailpipe of engine exhaust. It is suggested that before a gasoline additive is commercialized, an assessment on its PAH emission should be evaluated to make sure that the additive will not emit more PAHs and cause adverse effect on public health.
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PMID:Effect of the gasoline additives on PAH emission. 953 30

Scandium, gallium and vanadium contents in plants is on the ppm level, although plants from industrial areas can show higher concentrations of these elements. In Department of Analytical Chemistry of Silesian University there have been elaborated new, sensitive, spectrophotometric methods of determination of scandium, gallium and vanadium using Chrome Azurol S (CAS) and Sterinol (ST). The aim of this study was the application of these methods in analysis of cultivated plants from polluted regions. White cabbage from Upper Silesia was chosen. Because the spectrophotometric methods are not selective, scandium, gallium and vanadium should be preliminary separated from interfering elements. The solvent reaction was applied for the isolation from main and trace components of investigated material. Tienoiltrifluoracetone solution in xylene was used for the extraction of scandium, mesithyloxide for vanadium and n-butyl acetate--for gallium. Interfering and not separated Fe(III) was isolated using the extraction with acetylacetone solution in CHCl3 in the case of scandium and the reduction to Fe(II) by ascorbic acid in the case of gallium and vanadium. Due to influence of Fe(II) on the vanadium determination, KCN was used as a masking agent directly after the reduction. Scandium, gallium and vanadium were determined in 6 independent samples of white cabbage after dry or wet mineralization and contents of these leemnets were found from calibration graphs. Obtain results were checked by the internal standard addition method and Atomic Emission Spectrometry Method (ICP AES). The amounts of gallium and vanadium in white cabbage from Upper Silesia District determined by elaborated methods are in good correlation with a literature data, although the contents of vanadium are on the toxic level. The scandium concentration is higher than in plants from not industrial areas. The standard recovery is satisfactory. The Atomic Emission Spectrometry Method gave comparable results. The proposed the spectrophotometric methods are sensitive, precise and economical too, because they require only small amounts of reagents and simple not expensive apparatus. The methods can be recommended for many laboratories to the analytical control of white cabbage and after adaptation to the other plant material analysis.
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PMID:[Spectrophotometric determination of scandium,gallium and vanadium in white cabbage leaves]. 956 4

To study the health effects of high dietary maternal selenium intake breast milk, blood and toe-nails were collected from 143 women (20-24 days of lactation) living in Venezuelan states of Yaracuy and Portuguesa. Depending on the regional selenium intake level three regions were defined within the total range of 90-980 microgram per day. The samples were analyzed by means of INAA for the determination of trace elements, including selenium and zinc. The significant inverse correlation between Se and Zn in breast milk found in former studies was confirmed. Investigation of the Zn-binding pattern in milk whey was carried out by an on-line combination HPLC (SEC) for protein separation and ICP-AES for element detection. Six Zn-binding compounds including citrate were detected. A highly significant negative correlation was found between the citrate, which is the main low-molecular Zn-binding compound, and the maternal daily selenium intake. We determined that the decrease in zinc concentration is due to a decrease in the citrate level, which depends on the selenium concentration in breast milk. The selenium concentration in breast milk is, in turn, proportional to the dietary intake. In addition, significant changes in the UV- and Zn-profiles were observed in the milk whey with the highest selenium content, indicating that above a certain maternal intake level substantial changes in the composition of mammary secretory cells occur. This effect can be of interest for estimation of the safe dietary intake level of selenium.
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PMID:Maternal selenium status influences the concentration and binding pattern of zinc in human milk. 957 70

Hydrolysis of N-succinyl-L,L-diaminopimelic acid by the dapE-encoded desuccinylase is required for the bacterial synthesis of lysine and meso-diaminopimelic acid. We have investigated the catalytic mechanism of the recombinant enzyme from Haemophilus influenzae. The desuccinylase was overexpressed in Escherichia coli and purified to homogeneity. Steady-state kinetic experiments verified that the enzyme is metal-dependent, with a Km for N-succinyl-L,L-diaminopimelic acid of 1.3 mM and a turnover number of 200 s-1 in the presence of zinc. The maximal velocity was independent of pH above 7 but decreased with a slope of 1 below pH 7. The pH dependence of V/K was bell-shaped with apparent pKs of 6.5 and 8.3. Both L,L- and D,L-diaminopimelic acid were competitive inhibitors of the substrate, but d,d-diaminopimelic acid was not. Solvent kinetic isotope effect studies yielded inverse isotope effects, with values for D2OV/K of 0.62 and D2OV of 0.78. Determination of metal stoichiometry by ICP-AES indicated one tightly bound metal ion, while sequence homologies suggest the presence of two metal binding sites. On the basis of these observations, we propose a chemical mechanism for this metalloenzyme, which has a number of important structurally defined homologues.
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PMID:Hydrolysis of N-succinyl-L,L-diaminopimelic acid by the Haemophilus influenzae dapE-encoded desuccinylase: metal activation, solvent isotope effects, and kinetic mechanism. 967 18

The quantitative determination of Gd-containing magnetic resonance imaging (MRI) contrast agents in animal tissues is performed by both ICP-AES and ICP-MS. While ICP-AES has been used to determine Gd-containing contrast agents by other workers, no published methodology has been found. An accurate and precise method using nitric acid and microwave digestion for sample preparation is described. Dosed rat tissue, blood and plasma were measured by both ICP-AES and ICP-MS. The ICP-AES method is excellent for screening Gd levels and quantitative determination of concentrations above 400 ng ml-1, but it lacks the sensitivity to measure agent concentrations in low dose MRI studies. This work demonstrates that ICP-MS has the needed sensitivity to replace radiotracer methods currently used for low dose studies, while maintaining the accuracy and precision of results obtained by ICP-AES. Gadolinium detection limits in tissue were 0.04 mumol of Gd per kg of tissue, an order of magnitude lower than studies using radiotracer techniques.
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PMID:Gadolinium determination in tissue samples by inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry in evaluation of the action of magnetic resonance imaging contrast agents. 968

23 elements (Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, Hg, K, Li, Mg, Mn, Mo, Na, P, Pb, S, Ti, V, Zn) were measured in lady's thistle (Silybum marianum L.) herba and fructus by ICP-AES technique after digestion in teflon vessels. This is the first report about the content of these elements in the plant originated from Hungary. This measurements is important in view of plant physiology and pharmacology. Significant amounts of aluminium and iron were measured in lady's thistle herba. In the course of tea making, the relative concentration of some elements decreases because of the poor solubility of the compounds of these elements. The low concentration of these elements in teas in favourable in pharmacological aspect. No significant differences were found in boron, calcium, potassium and magnesium concentrations of lady's thistle fructus samples of different origin.
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PMID:[Determination of 23 elements in lady's thistle (Silybum marianum L. Gaertner)]. 970 2

The aim of this work was twofold: to study the binding pattern of trace elements in formulas as compared with breast milk and the relationship between trace elements in breast milk and in maternal dietary intake. To investigate the binding form of trace elements in these nutritive fluids, methods for protein separation were combined with methods for trace element determination in the eluted fractions. HPLC and ICP-AES or ICP-MS were coupled on-line for the simultaneous speciation of elements of nutritional interest, viz., Ca, K, Mg, P, S, Co, Cu, Fe, I, Mn, Mo, Se and Zn, and also the heavy metals Cd and Pb in both human mild whey and formulas. In order to minimize interactions between the labile metal protein complexes and the column material, size-exclusion chromatography was used for protein separation. The binding pattern of trace elements in formulas is significantly different from that in breast milk and depends on its main component (cow's milk or soy), its processing (hydrolysis) and the chemical form (inorganic) of the added compounds. For example, compared with breast-fed infants the iron supply of formula-fed infants is much higher (up to 20-fold); in addition, the binding forms of Fe are very different in the two fluids. This has to be evaluated with respect to interactions with other elements during intestinal uptake. The investigation of breast milk samples from different regions of the world showed comparable shapes for teh elution profiles and for Mo and Se a dependence on the regional maternal dietary intake. Speciation studies carried out on breast milk samples as a function of the selenium content showed significant changes in the zinc-binding pattern. In particular, citrate (as a zinc-binding component) was found to decrease with increasing dietary selenium intake of the mother.
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PMID:Speciation as an analytical aid in trace element research in infant nutrition. 970 76


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