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A newly devised, very accurate ("definitive") method for the determination of trace amounts of cobalt in biological materials was validated by the analysis of several certified reference materials. The method is based on a combination of neutron activation and selective and quantitative postirradiation isolation of radiocobalt from practically all other radionuclides by ion-exchange and extraction chromatography followed by gamma-ray spectrometric measurement. The significance of criteria that should be fulfilled in order to accept a given result as obtained by the "definitive method" is emphasized. In view of the demonstrated very good accuracy of the method, it is suggested that our values for cobalt content in those reference materials in which it was originally not certified (SRM 1570 spinach, SRM 1571 orchard leaves, SRM 1577 bovine liver, and Czechoslovak bovine liver 12-02-01) might be used as provisional certified values.
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PMID:Accurate determination of cobalt traces in several biological reference materials. 771 Aug 79

A high performance liquid chromatography (HPLC) with isocratic ion-pair-reversed-phase separation and simultaneous UV-detection at 232 nm and 292 nm is proposed as a method for the simultaneous determination of uric acid and creatinine in serum. The only sample preparation required is an appropriate dilution with the eluent and membrane filtration on non-adsorbent 0.2 micron membrane-filtration-devices. The inaccuracy of the method has been determined for NIST-SRM-909 (n = 10) and was + 0.5% for creatinine as well as for uric acid. The imprecision in this case was 0.8% for both analytes. The within-run imprecision for creatinine/uric acid was 0.4-0.5%/0.2-0.4% in the case of standards and 0.6-0.8%/0.4-0.7% in the case of serum-pools. The between-run imprecision for creatinine/uric acid obtained from serum pools was 0.8-1.1%/0.7-1.0%. The results for creatinine have been compared to those from an isotope dilution-gas chromatography-mass spectrometry using [13C, 15N2]creatinine as internal standard and selected mass detection at m/e = 329 and m/e = 332. The results for uric acid have been compared to an HPLC-method published previously (Kock R et al. J Clin Chem Clin Biochem 1989; 27:157-62). The method comparisons (n = 55) for the new combined method presented versus the reference method for creatinine and the candidate reference method for uric acid resulted in coefficients of correlation of r = 1.000 for both analytes. The new combined method presented is useful for the analysis of patient samples where the classical photometric procedures do not give reliable results, as often observed in monitoring after transplantation surgery.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:A method for the simultaneous determination of creatinine and uric acid in serum by high-performance-liquid-chromatography evaluated versus reference methods. 775 38

A microbiological assay to detect different chemical compounds of selenium for potential future use in the study of the distribution of these chemical forms in foods is being developed. This assay is based on the detection, by infrared analysis, of CO2 in a culture of Escherichia coli when the bacteria are grown in the presence of various selenium compounds. The CO2 production is the result of selenium-dependent formate dehydrogenase activity, which catalyzes oxidation of formic acid produced during glucose metabolism. Smooth response curves were generated over several orders of magnitude for selenocystine, selenite, and selenomethionine. The assay detects selenium concentrations (above background) as low as 1.5 nM for selenocystine and selenite and 4 nM for selenomethionine in minimal medium. Detection of selenomethionine was enhanced (to a sensitivity of 1.5 nM) by the addition of methionine to minimal medium and was enhanced even further (to a sensitivity of 0.8 nM) by the addition of a defined mixture of amino acids. Selenomethionine could be assayed in the presence of an amino acid concentration which is proportional to the amino acid/elemental selenium ratio found in a wheat gluten reference material (NIST SRM 8418). This implies that the assay can detect selenium compounds in a variety of foods at low concentrations, avoiding the background CO2 production caused by high concentrations of non-selenium-containing amino acids. The observation that methionine enhanced selenomethionine availability for formate dehydrogenase synthesis supports studies in animals demonstrating that methionine controls selenomethionine incorporation into selenoenzymes.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:Optimization of an Escherichia coli formate dehydrogenase assay for selenium compounds. 781 Oct 71

A method was developed to analyze various calcium supplements for Ca and Pb content. The analysis involves a dry ash of the supplements followed by wet digestion. The Pb is determined by graphite furnace atomic absorption spectrophotometry (GFAAS). Analysis of Ca is by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Ca supplements fortified with Pb at levels ranging from 0.25 to 10.0 micrograms/g yielded recoveries ranging from 82.7 +/- 4.2 to 105.0 +/- 1.7%. To test accuracy, the method was applied to National Institute of Standards and Technology standard reference materials (NIST SRMs) 1572 citrus leaves and 1486 bone meal. GFAAS analysis of SRM 1572 averaged 13.1 +/- 0.6 micrograms Pb per g (certificate value, 13.3 +/- 2.4 micrograms Pb per g), and analysis of SRM 1486 averaged 1.34 +/- 0.11 micrograms Pb per g (certificate value, 1.335 +/- 0.014 micrograms Pb per g). ICP-AES analysis of SRM 1572 averaged 3.12 +/- 0.01% Ca (certificate value, 3.15 +/- 0.10% Ca by weight), and analysis of SRM 1486 averaged 27.63 +/- 0.27% Ca (certificate value, 26.58 +/- 0.24% Ca). The method's limit of quantitation (LOQ), on supplement Ca basis and a 1 g sample, averaged 0.75 micrograms Pb per 1 g Ca for supplements containing 9 to 35% Ca by weight. At a Pb level of 0.663 micrograms/g Ca, the reproducibility relative standard deviation (RSDr) averaged 7.3% and the repeatability relative standard deviation (RSDR) averaged 8.0%. It is recommended that the method be studied collaboratively.
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PMID:Analysis of calcium and lead in calcium supplements by inductively coupled plasma-atomic emission spectrometry and graphite furnace atomic absorption spectrophotometry. 795 Apr 30

Electrothermal atomic absorption spectrometry with a temperature-stabilizing platform and palladium(II) nitrate-magnesium nitrate-barium nitrate matrix modifier combination was used to measure total selenium concentrations in 0.5-ml samples of human urine. The method was validated by analysis of desiccated, standard urine samples (SRM 2670) from NIST. The peak height response was linear from 0 to 150 micrograms Se/liter urine with a sensitivity of 0.001 absorbance unit/micrograms Se/liter and a detection limit of 6 micrograms Se/liter (P = 0.05) for a single measurement. Total urinary selenium concentrations and urine volumes of 24-h samples from 28 healthy adult subjects on self-selected diets and living in San Angelo, Texas were measured. Daily total urinary excretions of 16 male and 12 female subjects (mean +/- SD) were 28 +/- 26 and 34 +/- 25 micrograms Se/day, respectively. A single subject taking 300 micrograms Se/day in the form of aqueous SeO2 as a dietary supplement excreted 232 micrograms Se/day. The unsupplemented subjects' daily selenium excretions correspond to a mean dietary intake of approximately 60 micrograms/day.
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PMID:Palladium(II), magnesium(II), and barium(II) nitrate combinations for matrix modification in electrothermal atomic absorption measurement of total selenium in human urine. 797 75

On the base of literature the problems concerning the intralaboratory and interlaboratory quality assurance for analytical laboratories were discussed. The special attention was given on the role of standard reference materials (SRM's) in food and nutrition analysis and participation in the interlaboratory proficiency testing. The lists of some international recognised producers of certified reference materials and some SRM's for trace elements in food and water were also presented in this paper.
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PMID:[Quality assurance for analytical laboratories]. 801 32

Concentrations of Tin (Sn) were determined in botanical, dietary and biological reference materials (RMs), and in human livers from Japanese and American subjects using atomic absorption spectrophotometry (AAS) and neutron activation analysis (NAA), either in the instrumental mode (INAA) or in the radiochemical mode (RNAA). The mean Sn concentrations (+/- 1 S.D.) found in various RMs are: total diet (NIST SRM-1548) 3.57 +/- 0.52 and 3.61 +/- 0.52 microgram/g by AAS and INAA, respectively; non-fat milk powder (NIST SRM-1549) 2.5 +/- 1.4 ng/g and 1.9 +/- 0.3 ng/g; bovine liver (NBS SRM-1577) 18 +/- 2 and 20 +/- 0.3 ng/g; and citrus leaves (NIST SRM-1542) 0.25 +/- 0.02 and 0.243 +/- 0.006 microgram/g by AAS and RNAA, respectively. These comparisons demonstrate good agreement between the two methods. In apple leaves (NIST SRM-1515) and peach leaves (NIST SRM-1547), the measured concentrations by AAS were 77.1 +/- 20 and 85 +/- 15 ng/g; interferences by 160Tb did not permit an accurate assessment by INAA at this concentration. The Sn results obtained for the American human liver specimens by RNAA ranged from 0.135-0.712 microgram/g wet weight, and the Sn concentrations in Japanese human liver specimens determined by AAS ranged from 0.078-1.122 microgram/g wet weight in 23 individuals. The results from this study show that it is feasible to use INAA/RNAA and AAS in combination to establish recommended values in RMs.
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PMID:Determination of tin in biological materials by atomic absorption spectrophotometry and neutron activation analysis. 801 37

The National Institute of Standards and Technology (NIST, formerly the National Bureau of Standards) has developed and certified a Standard Reference Material, SRM 2381, for use in testing for bias in determinations of morphine and codeine in human urine. Each unit of this SRM consists of three vials with different levels of morphine and codeine in lyophilized urine. Three different analytical methods, employing GC/MS, LC/MS, and MS/MS, were used to certify the concentrations of each analyte. Results from the three methods were in good agreement and, therefore, were statistically combined to yield certified values of 138, 293, and 578 ng/mL for morphine and 134, 283, and 591 for codeine. A round-robin study on this material among nine military laboratories demonstrated the suitability of the SRM for its intended purpose.
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PMID:The certification of morphine and codeine in a human urine standard reference material. 812 93

The possible quantitative methods calculating safety limits for nutrient intakes are related conceptually to those used to calculate safe limits for exposure to environmental chemicals and to the therapeutic index used to assess the relative safety of drugs. The impact of using a fixed SF has been compared with the use of variable SFs. Of the methods identified, the SRM gives lower limits than does the MPM. However, neither of these methods calculates safety limits below the RDA, even for nutrients with narrow margins of safety. The acceptability criteria for toxicity data for use in identifying safety limits are an issue of major importance and must be resolved before calculated limits may be used to support policy or regulatory decisions. An advantage of adopting a standard formula involving systematically varying SFs to calculate safety limits is that the margin of safety below the expected range of toxicity for each nutrient would be systematic, without having the safety limit for any nutrient regress below its RDA. Once the data acceptability criteria were met, the safety limit would be identified objectively. The confidence in and reasonableness of safety limits, regardless of the method used to define them, will be enhanced if the objectives, data criteria, and the quantitative method have been agreed upon ahead of time by groups responsible for nutrition and health policy. Even with such agreement, the confidence in using such procedures to support policy decisions will be improved by the extent and quality of the data base on toxicity and adverse reactions associated with consumption of excessive levels of the nutrients under consideration.
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PMID:Safety limits for nutrient intakes: concepts and data requirements. 824 22

An on-line anodic stripping voltammetry (ASV) flow system, interfaced with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICPMS) detectors, has been used for determination of arsenic(III) and selenium(IV) and for elimination of polyatomic interferences which arise from chloride in sample matrices. Details of the working electrode preparation are discussed. Arsenic signals in ICP-AES were enhanced by as much as 10 times through preconcentration of sample volumes up to 5 mL. Using ICP-AES detection, recoveries for analyte spikes in 1:10 diluted urine were 102% for As(III) (matrix-matched standards) and 91% for Se(IV) (standards in electrolyte). Using ICPMS detection, determination of certified Se(IV) and Se(IV) spikes in diluted NIST SRM 2670 elevated urine gave recoveries of 92-103%, while recoveries of As(III) spikes in diluted NIST SRM 2670 urine ranged from 94 to 113%. High levels of chloride matrix exhibited little effect on the arsenic signal with ICP-AES or ICPMS detection. Elimination of the polyatomic interference ArCl+ in ICPMS was very efficient for diluted NIST SRM 2670 urine and for a synthetic matrix of 1000 micrograms/mL chloride.
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PMID:Determination of arsenic(III) and selenium(IV) using an on-line anodic stripping voltammetry flow cell with detection by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry. 829 28


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