An evaluation of thermal and epithermal neutron activation analysis compton suppression methods for biological reference materials

For neutron activation analysis (NAA), the usual matrix problems of sodium, chlorine, and bromine are well known to give rise to high backgrounds that inhibit the determination of several trace elements for short-lived or medium-lived NAA. For long counting times in long-lived NAA, very low backgrounds are required to achieve good sensitivities. We have investigated the use of thermal and epithermal NAA in conjunction with Compton suppression to determine several elements such as arsenic, antimony, cadmium, and mercury, at the level of a few nanograms. The values of these techniques are discussed in contrast to the standard radiochemical methods.     

RNAA as compared to ICP-MS for the analysis of normal human serum

The merits of radiochemical neutron activation analysis (RNAA) and inductively coupled plasma mass spectrometry (ICP-MS) are critically discussed for the determination of trace and ultratrace elements in normal human serum. For RNAA, two semiautomated procedures, allowing the determination of up to 18 elements, are briefly described. ICP-MS has a series of interesting features for the determination of trace elements. Matrix and spectral interferences can mostly be avoided or corrected for. After a simple 5- or 10-fold dilution and addition of an internal standard, more than 20 elements can be measured precisely and accurately.     

Factors affecting the levels reported for vanadium in human serum

Chemometric techniques may be applied to extract significant analytical information from a series of publications that present methods and results for determining trace elements in biological material. This approach was applied to the total of 28 papers published in 1971–1988 that reported determination of vanadium in normal human serum or plasma; the levels spanned four orders of magnitude. The most important factors affecting the analytical results were found to be the choice of analytical method and the experience of the laboratory in trace-element research. Results from the most experienced laboratories with the best analytical methods were found to be correlated with the precision of the data, indicating that the correct concentration of vanadium would be<1 mg/m³. This is in agreement with results subsequently obtained by radiochemical neutron activation analysis of eight samples of serum from Danish colleagues.     

Concentration of rare earth elements,As, and Th in human brain and brain tumors,determined by neutron activation analysis

Toxic elements As and Th, six rare-earth elemental profiles of brain tumor tissues from 16 patients of astrocytomas (grade I–III), and normal human brain tissues of 18 male, age-matched autopsies serving as controls have been studied by radiochemical neutron activation analysis. P-204 [di(2-ethylhexyl) phosphate] extraction chromatography column was used for group separation of rare-earth element (REE) by one step. Compared with the normal brain tissues, the analytical results showed that the concentrations of Th, La, Ce, Gd, and Lu were significantly higher in tumor tissues (P<0.01 or 0.001). The possible effects of REE on tumor cell were discussed.     

Neutron activation analysis for the determination of trace elements in biological materials

Biological Trace Element Research - Neutron activation analysis, in both its radiochemical and instrumental forms, is a precious technique for the determination of trace elements in biological...     

Changes of concentrations of the elements Co,Cr, Sb,and Sc in tissues of persons with joint implants

Elevated levels of Co and Cr were found in several organs of deceased implant bearers (CoCr-alloy/polyethylene joint prostheses) by means of instrumental and radiochemical neutron activation analysis as compared to normal persons. For comparative purposes, concentrations of the elements Co, Cr, Sb, and Sc were measured in heart, kidney, liver, and spleen of the patients and normal persons. For Cr determination, a new radiochemical separation technique with sufficiently low determination limit was employed. The importance of such investigations for studying possible carcinogenic effects of corrosion products and wear particles of metallic prostheses is mentioned.     

Assay for 2-oxoglutarate decarboxylating enzymes based on the determination of [1-14C]succinate: application to prolyl 4-hydroxylase

A method for the assay of 2-oxoglutarate decarboxylating enzymes based on determination of the reaction product [1-14C]succinate after precipitation of remaining 2-oxo[5-14C]glutarate with 2,4-dinitrophenyl hydrazine is reported. It is particularly useful for the study of the 2-oxoglutarate-coupled dioxygenase prolyl 4-hydroxylase (EC 1.14.11.2); it is superior to previously described assay methods of this enzyme with respect to simplicity of the procedure, speed, cost, and radiochemical safety. The results are highly reproducible, the standard deviation of repeated measurements being about 2% of the mean. The commercially available 2-oxo[5-14C]glutarate used in this study contained approximately 3% of radioactivity coeluting with succinate in HPLC and 1.5% of an unidentified radioactive compound as impurities, which contributed to the background.     

Trends in trace element determinations in blood,serum, and urine of the dutch population,and the role of neutron activation analysis

A critical review on the quality of literature data on trace elements in human blood, serum, and urine of inhabitants in the Netherlands has shown that many of the currently available data have been established 15–20 years ago. Only in a few publications are quality indicators mentioned, which should be considered typical—and minimal —for studies resulting at reference values. The use of neutron activation analysis for determination of trace elements in human body fluids was restricted to a few studies in the 1970s. However, although it is frequently assumed that the sensitivity of NAA might be insufficient, it is demonstrated that modern, large, well-type Ge detectors may serve well for the determination of trace elements in human body fluids via radiochemical NAA, for example.     

微波消解- 火焰原子吸收光谱法测定蜂胶中金属元素含量

目的:测定一种原产地为加拿大的蜂胶中金属元素的含量,为进一步研究蜂胶营养价值提供数据,同时改进测量方法。方法:用微波消解法处理样品,用硝酸和过氧化氢的混合物作为消解剂进行微波消解,并优化消解条件,然后用火焰原子吸收光谱法测定蜂胶制品中钙、铁、镁、锌、钠、钾、铜的含量。结果:七种元素相对标准偏差为0.85%~2.33%(n=7),回收率在96.5%~104.7%之间。试验结果表明该蜂胶中含有丰富的金属元素,且与河南产蜂胶相比,加拿大产蜂胶中多种金属元素含量远低于河南产蜂胶。结论:使用本文方法测定蜂胶中的金属元素含量,结果准确,方法可靠。为进一步探讨蜂胶制品金属元素与其保健功能的关系提供了有用数据。     

微波消解－火焰原子吸收光谱法测定蜂胶中金属元素含量

目的：测定一种原产地为加拿大的蜂胶中金属元素的含量,为进一步研究蜂胶营养价值提供数据,同时改进测量方法。方法：用微波消解法处理样品,用硝酸和过氧化氢的混合物作为消解剂进行微波消解,并优化消解条件,然后用火焰原子吸收光谱法测定蜂胶制品中钙、铁、镁、锌、钠、钾、铜的含量。结果：七种元素相对标准偏差为O．85％～2．33％（n=7）,回收率在96．5％～104．7％之间。试验结果表明该蜂胶中含有丰富的金属元素,且与河南产蜂胶相比,加拿大产蜂胶中多种金属元素含量远低于河南产蜂胶。结论：使用本文方法测定蜂胶中的金属元素含量,结果准确,方法可靠。为进一步探讨蜂胶制品金属元素与其保健功能的关系提供了有用数据。     

Assays for amino acid decarboxylase enzymes using ion-exchange cartridges

A general radiochemical method for estimating the activity of amino acid decarboxylases is reported. This method utilizes ion-exchange cartridges to separate unreacted radiolabeled amino acid substrates from product amines, which can then readily be quantitated by liquid scintillation counting. The assay is simple, rapid, and more sensitive than standard 14CO2 trapping procedures if uniformly labeled amino acid substrates are utilized. Acidic, basic, and aromatic amino acid decarboxylases can be assayed with the appropriate choice of cation or anion exchangers. The utility of the method is demonstrated for aspartate-alpha-decarboxylase, tyrosine decarboxylase, and lysine decarboxylase where kinetic parameters are comparable to values obtained by standard radiochemical 14CO2 trapping assays.     

稀土抗菌效应及应用的研究进展

稀土元素具有多种生物效应, 除了对农作物的增产作用外, 在医药方面还具有抗菌的作用, 近年来, 不少学者针对稀土元素的抗菌效应展开了相关的研究。本文介绍了稀土在抗菌领域的研究及应用, 包括稀土化合物对微生物生长的Hormesis效应、稀土化合物与抗生素的协同作用、稀土配合物的合成、以及稀土在抗菌材料上的应用等几个方面的内容, 并对稀土化合物及其配合物的抗菌机理进行了探讨, 最后, 展望了稀土化合物及配合物在抗菌领域的应用前景及研究重要性。     

Determinations of subnanomole elemental levels by NAA and their possible impact on human health related issues

Neutron activation analysis (NAA) is an appropriate tool for the determination of trace elements in biological systems. The virtually blank-free NAA procedures fittingly complement precautions employed in sampling and sample preparation of biological matrices. Results from instrumental NAA procedures used to establish baseline values and time trends for elements in human tissues demonstrate the advantages as well as the limits of these procedures for nanomole and, in a considerable number of instances, subnanomole elemental levels. In addition, subnanomole mass fractions have been determined with extremely low limits of detection by employing NAA with radiochemical separations isolating very low levels of radioactivity from the matrix background. The elements reviewed in this article include Cr, Se, Pt, and others that have been determined by NAA at subnanomole levels in human tissues and body fluids and in biological macromolecules.     

Preliminary study of the distribution of the toxic elements As,Cd, and Hg in human hair and tissues by RNAA

In order to study the relationships between trace element concentrations of hair and internal body burdens, a radiochemical NAA technique has been used for determination of the elements As, Cd, and Hg in autopsy samples of liver, kidney-cortex, lung, and hair from 24 male persons who died by accident. High significant positive correlations were observed between the As concentration in hair and in kidney-cortex, and between Cd and Zn concentrations in kidney-cortex. The contents of Cd, both for lung and kidney-cortex, were related to the smoking habits of the subjects.

     

Validation of determination of lead (Pb) in blood by electrothermal atomic absorption spectrometry (ETAAS) on the basis of interlaboratory comparison data

ISO 15189 standard establishes a requirement to periodically revalidate analytical methods for the determination of trace elements like Pb in blood, as conditions change and technical advances are made. The aim of this study was to revalidate an electrothermal atomic absorption spectrometry (ETAAS) method for determination of Pb in blood over the microrange 25–35 μg/dL, on the basis of historical results of interlaboratory comparison programmes. Precision and inaccuracy were estimated by analysis of records of an external quality control programme for Pb (PICC-PbS). The precision and inaccuracy values obtained were both less than 5%, highly satisfactory in view of the validation requirement that precision and inaccuracy be less than 10%. These findings demonstrate the effectiveness of this new validation methodology, which does not require any disruption of the laboratory's routine activity, and which can be used even if the method in question has not been validated previously at that laboratory.     

Biosorption of lanthanum and samarium by viable and autoclaved mycelium of Botryosphaeria rhodina MAMB-05

The ascomycetous fungus, Botryosphaeria rhodina MAMB-05, secretes a (1→3)(1→6)-β-D-glucan, and the scaled-up production of this β-glucan results in large amounts of mycelial biomass being produced that represent a potentially cost-effective biosorbent for rare-earth elements. High sorption capacities for both La(III) and Sm(III) were demonstrated for viable and autoclaved lyophilized fungal mycelium. Fourier-transformed infra-red absorption spectra and the point of zero charge (PZC) were similar for the viable and inactive fungal mycelia. The rare-earth lanthanide elements (La and Sm) binding increased at initial pH values greater than 5.0, which was also observed for the PZC determination. The maximum La(III) uptake capacity was observed at lower amounts of La(III) ions in solution, decreasing from 100.0 to 25.3% when the initial lanthanide concentration increased from 15 to 100 mg/L. Lanthanide biosorption by B. rhodina MAMB-05 mycelia followed the Langmuir model, and the affinity of biosorbent functional groups was similar for La(III) and Sm(III).     

Minor and trace elemental contents of cancerous breast tissue measured by instrumental and radiochemical neutron activation analysis

Many minor and trace elements influence the permeability of cell membranes by competing for binding sites, and exert direct or indirect action on the carcinogenic process. Instrumental and radiochemical neutron activation analysis has been employed for the determination of more than 20 elements in normal and cancerous breast tissues of 6 patients. Most trace elements, viz., Zn, Cu, Mn, Co, Se, Br, As, Sb and Cd, are elevated in cancerous tissue, whereas lower levels are observed for Fe, Cs, I, and Sr. Similarly, concentrations of minor constituents, such as Na, K, P, Cl, and Mg, are enhanced compared to normal tissue. Several elements incorporate into the normal cell, change its enzymatic activity, and accelerate the growth of tumor.

     

Charged-particle activation analysis of biological material

Charged-particle activation analysis offers a number of interesting possibilities for the determination of trace elements in biological material. It allows the determination of those elements that are difficult or impossible to determine by neutron activation, such as Li, B, Al, Si, V, Cr, Ni, Cd, Sn, Tl, and Pb. Up to now, protons have been successfully applied to samples of both vegetale and human origin. A number of difficulties have to be overcome, one of which is excessive heating of the samples owing to the limited range of the charged particles, thus giving rise to a high energy deposition in a small volume. Moreover, the sample composition has to be known to allow the calculation of the range of the particles. an interesting alternative has been proposed using an internal standard together with a standard additions procedure. Proton activation analysis was tested on a wide variety of reference materials, giving evidence that accurate results can be obtained for many trace elements, even when applying a purely instrumental method. Thus, the method can also be applied in the certification of reference materials, since nuclear methods are independent of chemical properties of the sample.     

Teneurs en éléments majeurs et traces de spirulines (Arthrospira platensis) originaires de France,du Tchad,du Togo,du Niger,du Mali,du Burkina-Faso et de République centrafricaine

Data on mineral elements in spirulinas being limited, we analyzed macrominerals and trace elements of samples from France and Africa. Spirulinas cultivated in France have a composition in macromineral elements similar to those of the literature. The entire contents of trace elements are low. Unlike marine cyanobacteria, they do not concentrate rare-earth elements. Spirulina harvested in Chad has high levels in macrominerals and trace elements, due to traditional drying and harvesting methods. Rare-earth element levels are attributed to this pollution and not to their concentration in spirulinas, because rare-earth element normalized profiles of spirulina are strictly parallel to those of ouadis mud and very different from those of ouadis water. Despite the sometimes high content of total As, normal water consumption in Chad presents no health problems. Spirulinas grown in Togo, Niger, Mali, Burkina-Faso and Central African Republic have chemical compositions similar to those of Chad spirulinas, but with a lower content of macromineral and trace elements, reflecting a lower mineral pollution. Rare-earth element normalized patterns dismiss an aeolian pollution and the pollution is rather of pedological origin. They show no toxicity problem except spirulinas from Burkina-Faso, whose Pb content is too high. The variability of composition of spirulinas can be largely attributed to the mineral pollution of the samples. Significant levels of rare-earth elements sometimes found in the literature reflect this pollution.     

Potential limitations of recrystallization for the definitive identification of radioactive steroids

The usefulness of recrystallization in establishing the radiochemical purity of steroids is widely recognized, but the potential limitations of the technique have received little attention. The current study reports the failure of standard recrystallization procedures using methanol/water as the solvent pair to separate contaminating ¹⁴C-17-hydroxyprogesterone (17-hydroxy-4-pregnene-3, 20-dione) from ³H- and ¹⁴C-labeled 11-deoxycortisol (17,21-dihydroxy-4-pregnene-3,20-dione) despite ten serial crystallizations. The standard criteria of radiochemical purity were met despite gross impurity of the crystals as evidenced by thin layer chromatography. Thus, recrystallization may, under certain conditions, yield misleading results when employed as the only method for identifying radioactive steroids. These observations illustrate the importance of an optimal choice of solvent and crystallization conditions, and emphasize the need for confirmation by derivative formation and chromatography.