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[Selenium content of tea from different provinces of the People's Republic of China].

In the People's Republic of China there are wide regions where many people suffer from strong selenium deficiency. In order to elucidate the possibilities to compensate this state of need by the national drink, the selenium contents of 31 tea samples from nine provinces of the PR China were determined by hydride generation atomic absorption spectrometry (HG-AAS). The Se contents of the ten analyzed tea samples from one region with soils containing high selenium amounts range from 83 ng/g to 7530 ng/g. These results are in contrast to the Se contents of the remaining tea samples from other regions, which range from 28 to 573 ng/g. The extractable part of selenium in the tea drink ranges between 7% and 27% without significant difference among different tea samples. The accuracy of Se determination was tested by using one tea standard reference material. The daily consumption of one "Se tea" examined in this study assures that people who suffer from a Se deficiency resume enough of it. Drinking normal quantities of this tea an intoxication by Se is not to be expected.

China↗

Multielemental analysis of human fetal tissues using inductively coupled plasma-mass spectrometry.

Inductively coupled plasma-mass spectrometry (ICP-MS) was used to study the distribution of 26 major and trace elements in six tissues from 21 human fetuses aged 16-22 wk. Brain, lung, spleen, kidney, heart, and liver were analyzed following a microwave oven digestion step carried out according to clean techniques designed for ultratrace metal analyses. Precision and accuracy controls were conducted using standard reference material #1577b Bovine Liver. Significant differences among tissues were found for most of the elements. Essential trace elements seem to be increasingly retained as fetal tissues mature and become physiologically functional. The ranges of concentrations measured in fetal tissues at this stage of development are generally lower and much narrower than in adult tissues. The age of the fetus, which is not given in most studies, as well as the different techniques and levels of quality assurance could be responsible for the discrepancies in the trace metal concentrations reported here and in the literature. Intratissue homogeneity was also assessed in five human fetal brains. Frontal, occipital, parietal and temporal lobes, striatum, hippocampus, and thalamus were isolated and analyzed separately. No significant differences were found in the distribution of any of the elements at this stage of development. Because of the relatively narrow ranges of concentrations found for most elements, we believe that the results presented in this study represent the inorganic fingerprint of the main tissues of normal fetuses at midpregnancy for the Greater Montreal area.

Animals↗

Determination of trace boron in microsamples of biological tissues.

A benign-by-design method for the determination of boron (B) in microsamples of biological tissues was developed. This is a simple, automated, microdigestion method. Use of reagents and generation of waste are minimized, and the use of toxic/hazardous reagents is eliminated as compared to currently available B methodology. Microsamples are accommodated by the method; 100-400 mg samples were used in this study. B is determined by inductively coupled plasma atomic emission spectrometry (ICPAES) at 249.678 nm. The instrument detection limit for B is 0.01 microgram/mL. Interference studies have been investigated for 21 common elements. Over 250 analyses of standard reference materials were analyzed during the study duration. Recoveries for a series of biological tissues, both plant and animal, ranged from 82-104%.

Animals↗

Microwave digestion preparation and ICP determination of boron in human plasma.

A microwave digestion procedure, followed by Inductively Coupled Argon Plasma Spectroscopy, is described for the determination of boron (B) in human plasma. The National Institute of Standards and Technology (NIST) currently does not certify the concentration of B in any substance. The NIST citrus leaves 1572 (CL) Standard Reference Material (SRM) and wheat flour 1567a (WF) were chosen to determine the efficacy of digestion. CL and WF values compare favorably to those obtained from an open-vessel, wet digestion followed by ICP, and by neutron activation and mass spectrometric measurements. Plasma samples were oxidized by doubled-distilled ultrapure HNO3 in 120 mL PFA Teflon vessels. An MDS-81D microwave digestion procedure allows for rapid and relatively precise determination of B in human plasma, while limiting handling hazards and sources of contamination.

Argon↗

Neutron activation analysis of biological samples at the radiochemistry division of IPEN-CNEN/SP.

Neutron activation analysis is a very useful method for determination of a great number of elements in biological samples. At the Radiochemistry Division of the IPEN-CNEN/SP, this method is being extensively applied to study several materials, such as extracts from medicinal plants, human hair, snake venoms, human lungs, food-stuffs, and corn samples. Both instrumental neutron activation analysis (INAA) and radiochemical neutron activation analysis (RNAA) are used to analyze real samples, as well as biological standard reference materials to evaluate the accuracy and precision of the results.

Brazil↗

Neutron activation analysis of biological samples with a preirradiation chemical separation.

A preirradiation separation procedure has been developed to separate Al, Cu, Mn, and V from biological materials. Chelex-100 resin is used as the separation medium, and the resin is irradiated directly. Three NIST biological Standard Reference Materials and five samples of human blood serum, obtained under carefully controlled conditions, have been analyzed by NAA following this separation.

Blood Chemical Analysis↗

Radioisotope induced X-ray emission (RIXE) studies in life sciences.

The inherent advantages of radioisotope induced X-ray emission (RIXE) are briefly presented, with emphasis on their applications to analysis in the life sciences. The following selected applications by RIXE are discussed in general: (1) In vivo analysis: the determination of stable iodine in the thyroid and heavy metals in human bone; (2) the analysis of small tissue samples (about 10 mg) for the simultaneous determination of trace elements between 25 less than or equal to Z less than or equal to 40; data are given from a time study of the disease progress of Lewis lung tumor on a rat's liver over a 24-d period; and (3) a homogeneity study of iron, strontium, and zirconium in IAEA's SL-3 Lake sediment standard reference material is presented.

Animals↗

Investigation of the direct hydride generation nebulizer for the determination of arsenic, antimony and selenium in inductively coupled plasma optical emission spectrometry.

A direct hydride generation nebulizer (DHGN) was explored for introduction of the sample in inductively coupled plasma-optical emission spectrometry (ICP-OES) using radially viewed mode. This simple hydride generation system was constructed in our laboratory and requires similar plasma operating conditions to conventional nebulizer-spray-chamber arrangements. This work was focused on the optimization of the operating conditions for hydride generation and evaluation of the main analytical figures of merit for the determination of As, Sb and Se. The excitation conditions of the ICP-OES instrument operated with the DHGN were also explored. Results showed that the analytical performance of the new system for the determination of As, Sb and Se was superior to that of conventional nebulization systems. The DHGN also enabled the determination of elements that do not form volatile hydrides, but with less sensitivity than conventional nebulization systems. Evaluation of the plasma robustness showed that gases generated in hydride generation do not significantly affects the plasma discharge. Similar to conventional hydride generation techniques, analysis with DHGN was susceptible to non-spectroscopic interferences produced by transition metals. Finally, the utility of the DHGN in practical ICP-OES studies was demonstrated in the determination of trace elements in an oyster tissue standard reference material.

Animals↗

New NIST sediment SRM for inorganic analysis.

NIST maintains a portfolio of more than 1300 standard reference materials (SRM), more than a third of these relating to measurements in the biological and environmental fields. As part of the continuous renewal and replacement efforts, a set of new marine sediments has been recently developed covering organic and inorganic determinations. This paper describes the steps taken in sample preparation, homogeneity assay, and analytical characterization and certification with specific emphasis on SRM 2702 inorganics in marine sediment. Neutron activation analysis showed the SRM to be highly homogeneous, opening the possibility for use with solid sampling techniques. The certificate provides certified mass fraction values for 25 elements, reference values for eight elements, and information values for 11 elements, covering most of the priority pollutants with small uncertainties of only several percent relative. The values were obtained by combining results from different laboratories and techniques using a Bayesian statistical model. An intercomparison carried out in field laboratories with the material before certification illustrates a high commutability of this SRM.

Certification↗

Quality-control materials in the USDA National Food and Nutrient Analysis Program (NFNAP).

The US Department of Agriculture (USDA) Nutrient Data Laboratory (NDL) develops and maintains the USDA National Nutrient Databank System (NDBS). Data are released from the NDBS for scientific and public use through the USDA National Nutrient Database for Standard Reference (SR) ( http://www.ars.usda.gov/ba/bhnrc/ndl ). In 1997 the NDL initiated the National Food and Nutrient Analysis Program (NFNAP) to update and expand its food-composition data. The program included: 1) nationwide probability-based sampling of foods; 2) central processing and archiving of food samples; 3) analysis of food components at commercial, government, and university laboratories; 4) incorporation of new analytical data into the NDBS; and 5) dissemination of these data to the scientific community. A key feature and strength of the NFNAP was a rigorous quality-control program that enabled independent verification of the accuracy and precision of analytical results. Custom-made food-control composites and/or commercially available certified reference materials were sent to the laboratories, blinded, with the samples. Data for these materials were essential to ongoing monitoring of analytical work, to identify and resolve suspected analytical problems, to ensure the accuracy and precision of results for the NFNAP food samples.

Agriculture↗

Development of a murre (Uria spp.) egg control material.

The Seabird Tissue Archival and Monitoring Project (STAMP) is a collaborative Alaska-wide effort by the US Fish and Wildlife Service's Alaska Maritime National Wildlife Refuge (USFWS/AMNWR), the US Geological Survey's Biological Resources Division (USGS/BRD), the Bureau of Indian Affairs Alaska Region Subsistence Branch (BIA/ARSB), and the National Institute of Standards and Technology (NIST) to monitor long-term (decadal) trends in environmental contaminants using seabird eggs. To support this effort, a matrix- (seabird egg) and concentration-specific control material was needed to ensure quality during analytical work. Although a herring gull egg quality assurance (HGQA) material is available from Environment Canada (EC), contaminant concentrations in this material tended to be higher than those observed in Alaskan murre (Uria spp.) eggs. Therefore, to prepare a more appropriate control material, a total of 12 common murre (U. aalge) and thick-billed murre (U. lomvia) eggs from four Bering Sea and Gulf of Alaska nesting locations were cryohomogenized to create 190 aliquots each containing approximately 6 g. This new control material was analyzed by different methods at NIST and EC facilities for the determination of concentrations and value assignment of 63 polychlorinated biphenyl (PCB) congeners, 20 organochlorine pesticides, and 11 polybrominated diphenyl ether (PBDE) congeners. The total PCB concentration is approximately 58 ng g(-1) wet mass. Results obtained for analytes not listed on the certificates of analysis of the previously used control materials, HGQA and NIST's Standard Reference Material (SRM) 1946 Lake Superior Fish Tissue, are also presented.

Alaska↗

New low-index liquid refractive index standard: SRM 1922.

A new standard for the calibration of refractometers has been developed. Standard Reference Material (SRM) 1922 is a mineral oil with a refractive index nD = 1.46945 at 20 degrees C, which is within the range of the Brix scale (% sucrose). The change in refractive index with temperature (dn/dT) has been characterized for the range 15 degrees C to 35 degrees C to allow for calibrations within that range of temperatures. The refractive indices were measured at 5 wavelengths in the visible spectrum by using the method of minimum deviation with a +/- 2-3 x 10(-5) uncertainty at 20 degrees C. The values of nD and dnD/dT were determined by fits of a two-term Cauchy function to the values at the measured wavelengths with a +/- 6 x 10(-5) uncertainty in nD at 20 degrees C.

Calibration↗

Determination of Ca, Mg, Fe, Cu, and Zn in blood fractions and whole blood of humans by ICP-OES.

Inductively coupled plasma-optical emission spectrometry (ICP-OES) was applied to the determination of the elements Ca, Mg, Fe, Cu, and Zn in blood plasma, erythrocytes, lymphocytes, and whole blood to obtain reliable data on their distribution in blood fractions. The samples were carefully collected to avoid contamination. Two different nebulizers (Babington and Meinhard) were tested and optimized for this analytical problem. Line selections for all elements of interest were performed (LODs were 0.8 microg/L for Ca, 1.7 microg/L for Cu, 3.0 microg/L for Fe, 1.1 microg/L for Mg, and 4.2 microg/L for Zn). Recoveries were determined as approx. 100%, and standard reference material was analyzed to obtain reliable data on element distribution. The optimized method was applied to the determination of Ca, Mg, Fe, Cu, and Zn in the course of a clinical study on blood and blood fractions of two groups of humans of differing health. The concentrations measured in blood fractions were verified by balancing with the values found in whole blood.

Adult↗

Electrothermal atomic absorption spectrometric determination of cobalt in biological samples and natural waters using a flow injection system with on-line preconcentration by ion-pair adsorption in a knotted reactor.

An on-line flow injection preconcentration-ETAAS method is developed for trace determination of cobalt in biological materials and natural samples by ion-pair sorption on the inner walls of a PTFE knotted reactor. The ion-pair is formed between the negatively charged cobalt-nitroso-R-salt complex and the tetrabutylammonium counter-ion. An enhancement factor of 15, a sampling frequency of 17 and a concentration efficiency of 4 are obtained for a preconcentration time of 60 s and a sample loading flow rate of 5 mL min(-1). The detection limit (3sigma) is 5 ng L(-1). The relative standard deviation at the 0.2 microg L(-1) level is 2.3%. The analytical results obtained for standard reference materials are in good agreement with the certified or indicated values and satisfactory recoveries of spiked cobalt in tap water are obtained.

Animals↗

Lead in micro-samples of whole blood by Rhenium-cup in-torch vaporization-inductively coupled plasma-atomic emission spectrometry (ITV-ICP-AES).

A method is described for screening of lead in diluted micro-samples of whole blood by a Re-cup, in-torch vaporization (ITV) sample introduction system for inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method required minimum sample preparation. For example, blood was diluted with water and Triton X-100 in 0.5% HNO3 and, 5 microL were deposited on the Re-cup of the ITV sample introduction system. Samples were dried and charred in-situ prior to vaporization. Levels 1, 2, 3 and 4 (Pb concentration: 4.04, 10.3, 20.59 and 39.36 microg/dL) of NIST Standard Reference Material 955b 'lead in bovine blood' were used to test accuracy and precision. Accuracy was acceptable and precision was below 10% for levels 2-4 and 15% for level 1.

Animals↗

Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography mass spectrometry.

A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry. The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown.

Gas Chromatography-Mass Spectrometry↗

Ultrasound of intrinsic wrist ligament and triangular fibrocartilage injuries.

OBJECTIVE: The objective of this study was to evaluate ultrasound as a diagnostic tool for investigating scapholunate and lunatotriquetral ligamentous and triangular fibrocartilage (TFC) tears. Ultrasound findings were compared to conventional arthrogram findings, as the reference gold standard. DESIGN AND PATIENTS: In total 26 patients, 17 males and 9 females ranging in age from 17 to 35 (mean age, 34), were evaluated on referral for investigation of wrist pain. All patients were examined by high resolution ultrasound, using a 9-13 MHz transducer. All wrist ultrasound examinations were also compared to conventional tricompartmental arthrography, as the diagnostic gold standard reference. RESULTS: All ten scapholunate tears confirmed on arthrography were detected on ultrasound. Two of 8 lunatotriquetral and 7 of 11 TFC tears were correctly diagnosed on ultrasound. Sensitivity of ultrasound diagnosis ranged from 25% for lunatotriquetral tears to 100% for scapholunate tears. No false positive results were recorded for any of the three examined structures. CONCLUSION: The study results suggest that sonography is accurate for scapholunate tears, but is not accurate for evaluation of lunate-triquetral tears. It has intermediate accuracy for triangular fibrocartilage tears.

Adolescent↗

Determination of cadmium levels in agricultural areas of Carşamba and Bafra plains.

Cadmium pollution resulted from fertilizer applications were studied by determining cadmium levels in agricultural and non-agricultural soils of Bafra and Carşamba plains. Soil samples of 68 were collected from agricultural (34) and non-agricultural (34) areas. The sample of 2 g was placed in a test tube and digested with hydrochloric acid and nitric acid mixture (3:1, v/v) in an aluminum block. Taking up the evaporated residue was dissolved in 1% nitric acid and total cadmium concentrations were determined with GF-AAS. Mean level of cadmium contents were found in agricultural areas 0.162 +/- 0.078 for Carşamba and 0.433 +/- 0.288 mg kg(-1) for Bafra. The accuracy of the method was tested with determining cadmium contents of standard reference material and cadmium spiked soil samples.

Agriculture↗