Neutron activation analysis of the NIST Bovine Serum Standard Reference Material using chemical separations

Summary The US National Institute of Standards and Technology is currently in the process of certifying a Bovine Serum Standard Reference Material. In addition to elements normally considered to be of clinical interest, a number of other elements, which are analytically more difficult to determine yet are of importance from either a nutritional or toxicological viewpoint, are being determined by a variety of analytical techniques. Neutron activation analysis in combination with appropriate pre- or post-irradiation chemical separations, has been used to determine many of these difficult elements.

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Neutronenaktivierungsanalyse des Standardreferenzmaterials NIST Bovine Serum mit Hilfe chemischer Trennungen

     

Characterization (certification) of Bovine Muscle Powder (NIST RM 8414), Whole Egg Powder (NIST RM 8415) and Whole Milk powder (NIST RM 8435) Reference Materials for essential and toxic major, minor and trace element constituents

Summary Bovine Muscle Powder (NIST RM 8414), Whole Egg Powder (NIST RM 8415) and Whole Milk Powder (NIST RM 8435) Reference Materials were characterized for essential and toxic major, minor and trace element composition in an interlaboratory cooperative characterization campaign. Extensive application of widely varied analytical methods yielded best estimate concentration values for 27, 23 and 21 elements, and informational concentration values for 5, 4 and 9 elements, respectively, in RM's 8414, 8415 and 8435. These Reference Materials are intended for analytical quality control of element determinations on meat, egg and milk-based products as well as agricultural/food materials with related matrices.Contribution no. 92–147 from Centre for Land and Biological Resources Research     

NAA characterization of the new Bovine Liver SRM

The National Institute of Standards and Technology (NIST) is preparing a freeze-dried powdered bovine liver tissue Standard Reference Material (SRM) to replace SRM 1577b Bovine Liver as the stock of this material was exhausted during 2006. Like the original SRM 1577 issued in 1972, this renewal focuses on the key elements for diagnostic, nutritional, and toxicological measurements that are important to medical, veterinary, and environmental sciences investigations. NIST’s approach for value assignment included extensive characterization by neutron activation analysis (NAA). Difficulties in the determination of some elements present at very low levels were overcome by use of radiochemical separations. Twentyone elements were characterized in SRM 1577c by NAA. The previous materials, SRM 1577 and 1577b, served as quality control.     

高效液相色谱分离牛胸腺多肽的研究

本文以不同色谱方法对牛胸腺多肽进行了分离,寻求出能对牛胸腺多肽得到满意分离的色谱条件。     

Czechoslovakian biological certified reference materials and their use in the analytical quality assurance system in a trace element laboratory

Summary The Trace Element Laboratory of the University of Agriculture in Prague (CSFR) participated successfully in interlaboratory experiments on the determination of the contents of trace elements in seven Czechoslovakian reference materials. Czechoslovakian certified reference material CRM 12-02-01 (Bovine liver) was used for the development of a new analytical method using the Dry Mineralizer Apion as well as in analytical quality assessment of data in the determination of Cd, Pb, and Hg contents in routinely analyzed animal tissues.     

Microwave digestion of biological samples with tetramethylammonium hydroxide and ethylenediaminetetraacetic acid for element determination

A microwave-digestion system with a closed PTFE vessel was used to improve the leaching of inorganic constituents from biological samples with tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacetic acid (EDTA). The effects of microwave parameter settings and the quantities of TMAH and EDTA used on leaching efficiency were evaluated. This new digestion method has been applied to the standard reference materials NIST SRM 1577 B Bovine Liver 1515 Apple Leaves and NIES CRM No. 1 Pepperbush, No. 3 Chorella, No. 6 Mussel and No. 7 Tea Leaves. The major and minor elements in the digests were analyzed by flame atomic absorption spectrometry or graphite furnace atomic absorption spectrometry. Good agreement of the analytical results with the certified values was obtained.     

Bovine reference materials for accuracy control of blood lead analysis

Summary There is a lack of suitable commercially available reference materials for controlling the accuracy of determinations of trace elements in body fluids. This is a particular problem with blood lead measurements where results on individual patients or findings of population surveys may have major clinical, environmental or economic implications.Bovine blood haemolysate surrogate reference materials for internal accuracy control of blood lead measurements have been used systematically over the past decade by the SAS Trace Elements Sub-group in Britain. They have also been used by participating laboratories in the European Community Screening Programme for blood lead in an effort to harmonise the data.The seven SAS laboratories have collaborated in assigning values for blood lead concentration to three specially prepared batches of bovine reference materials between 1984 and 1987. The results show that it is possible for a small group of specialist laboratories to accurately and reproducibly assign values for reference materials in this way, so as to be suitable for use in internal accuracy control. Moreover, it has been possible to demonstrate the stability of the materials over a two-year period. This procedure offers a useful model for improving the accuracy of other assays of clinical interest.

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Rinder-Referenzmaterialien zur Richtigkeitskontrolle von Bleianalysen in Blut

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Presented on behalf of the Trace Elements Sub-group of the Supraregional Assay Service (SAS) of the U.K. National Health Service     

Determination of copper, iron, manganese, lead and cadmium in automatically wet-digested animal tissue by graphite-furnace atomic-absorption spectrometry with zeeman background correction

An efficient wet digestion method is described which allows the determination of various elements in animal tissues. Copper, iron, manganese, lead and cadmium in one dilution of the digested sample can be determined by means of graphite-furnace atomic-absorption spectrometry, with Zeeman background correction. Tests with the National Bureau of Standards Bovine Liver SRM as reference gave analytical results, obtained with calibration graphs as well as by the standard-addition method, which agreed well with the certified values.     

The Use of Bovine Serum Albumin as a Ligand in Affinity Chromatographic Clean-up of Non-Steroidal Anti-Inflammatory Drugs from Bovine Plasma

The European Union regulates the use of non-steroidal anti-inflammatory drugs (NSAID) in animal production and official national analytical monitoring programmes have been set up in each member state to detect residues of the drugs in bovine plasma. In this work, we describe the development and application of affinity chromatography for molecular recognition of NSAID in bovine plasma. Bovine serum albumin (BSA), the plasma protein which binds such drugs, was covalently bound to a polymeric support via its glycosyl moieties. Loading capacities and specificity were tested both on standard solutions and on spiked bovine plasma for nine drugs—ketoprofen, naproxen, phenylbutazone, oxyphenylbutazone, acetylsalicylic acid, salicylic acid, tolfenamic acid, diclofenac, and nimesulide—chosen as being the most representative of the different chemical sub-classes of NSAID. The BSA columns could bind up to 150 × 10^–6 g total of a mixture of these nine NSAID, with mean recoveries ranging from 74.0% (tolfenamic acid) to 96.0% (nimesulide). HPLC separation on an RP C₁₈ column with a linear gradient enabled resolution of the drugs; identification was achieved by coupling with photodiode array detection (DAD) operated at 240 and 280 nm. Results showed that all the compounds except acetylsalicylic acid were bound effectively by the BSA affinity columns. When plasma samples were spiked at 2.5 g mL^–1 with a mixture of the NSAID the chromatographic profile and UV spectra recorded (in the range 220–350 nm) indicated the procedure was sufficiently selective for identification of the drugs at the concentrations expected according to their pharmacokinetics. No memory effects and matrix interferences were observed.Revised: 18 December 2003 and 16 April 2004     

Use of multiwalled carbon nanotube disks for the SPE of some heavy metals as 8-hydroxquinoline complexes

A multiwalled carbon nanotube disk was used for the SPE of some toxic heavy metals from environmental samples. Metal ions were adsorbed on the disk as 8-hydroxquinoline complexes, then quantitatively desorbed from the disk by using 10 mL 2 M HNO3. The effects of analytical parameters, including pH, sample volume, and flow rates, on the recoveries of Cd(II), Co(II), Ni(II), Pb(II), Fe(III), Cu(II), and Zn(II) were investigated. The influences of some 1A and 2A group elements and some other ions as concomitant ions on the recoveries of analyte ions were also examined. The LODs of the presented preconcentration-separation system for the analyte ions were found to be in the range of 1.0-5.2 microg/L. In order to validate the procedure, SRM 1577B Bovine Liver, IAEA 336 Lichen, and HR-1 Humber river sediment certified reference materials were analyzed. The proposed method has been applied to the determination of understudy elements in some pharmaceutical samples and natural water samples from different sites in Turkey.     

Intercomparison and certification of some Chinese and international food and biological matrix CRMs for several uncertified ultratrace elements by NAA

Radiochemical neutron activation analysis was used for determinationsof 8 rare earth elements (La, Ce, Nd, Sm, Eu, Tb, Yb and Lu) in two ChineseCRMs, GBW 08503 (wheat) and GBW 09101 (hair), and Cs, Sr, Th and U in fiveNIST SRMs, 1548 (Total Diet), 1486 (Bone Meal), 8414 (Bovine Muscle), 1566a(Oyster Powder) and 1575 (Pine Needles). These determinations are for eventualcertification of above ultratrace elements so far not certified. The radiochemicalseparation scheme used in RNAA of NIST SRMs is an anion exchange followedby the co-precipitation by (REE)F 3 for U and Th, and a SrSO 4 precipitationfor Sr and Cs. For RNAA of the two Chinese CRMs, a one step (REE)F 3 precipitationwas used. Chemical yields were determined for all relevant elements by tracerexperiments. All these materials were also analyzed by ICPMS, that offeredan opportunity to compare the two major trace analytical techniques on theirmerits and drawbacks for these particular cases. RNAA is proven to be oneof the important techniques in ultratrace analysis, especially in certificationof some ultratrace elements. Determination of elements in sub-ng/g level isstill an area to be further investigated because: (1) some such elements areimportant in food and health related environmental studies, (2) many of theseelements have no (or very few) certified values in existing biological CRMs,(3) reliable techniques qualified for ultratrace analysis are needed to beestablished, and (4) sampling behavior of elements at these levels is stillnot very well known (recommended minimum sample size may not be adequate).     

Photoluminescence of crystallophosphors for the determination of 237Np and 239Pu

The photoluminescence of crystallophosphors, activated by neptunium and plutonium has been studied in connection with the necessity of discovering and elaborating on new analytical methods for actinides determination. Crystallophosphors on the base of fluorides, molybdates and tungstates have been prepared by introducing neptunium and plutonium solutions into the powder matrix, further drying and blend calcination. Luminescence spectra at room temperature have been found to have some broad bands in the near i.r. region independently of the method of crystallophosphor preparation, the oxidation state of introduced elements and the conditions of u.v. irradiation. The effect of matrix nature, flux content and concentration of quenching elements in analyzed solution on crystallophosphors luminescence has been studied. The methods of neptunium and plutonium     

Immobilization of Bovine Serum Albumin on Polytetrafluoroethylene for Application as a Potential Solid Support for Biosensor Development with Visual Detection

Immobilization of biomolecules on polymers is attractive for developing new biosensors and analytical methods. Polytetrafluoroethylene, PTFE (Teflon), is a low-cost polymer that has unique chemical and physicochemical properties. In this work, PTFE was investigated as a solid support for biosensor development. Bovine serum albumin (BSA) was immobilized directly on PTFE thin films without pretreatment. BSA was biotinylated, while the immobilization was controlled by the formation of visual spots using either streptavidin–fluorescein or streptavidin–gold nanoparticle conjugates. The visualization of the spots was accomplished by the naked eye (red spots) or a digital camera that captures the emitted fluorescence (green spots). The signal-to-background ratio was determined for both detection systems and was equal to 24.4 and 58.4 for streptavidin–fluorescein and streptavidin–gold nanoparticles, respectively.     

High-Performance Gel-Permeation Chromatography of Bovine Skim Milk Proteins

Abstract

The separation of bovine skim milk proteins by gel-permeation high performance liquid chromatography was examined. Toya-Soda TSK-GEL (Type SW) columns were used with an eluent of .05 M phosphate buffer (pH 6.80) containing .1 M sodium sulfate at .5 ml/min. Bovine whole milk was centrifuged to remove lipids, and the resultant skim milk directly injected. A 2000SW column yielded three protein peaks: 1 = casein, IgG and BSA; 2 = 6-lactoglobulins and BSA; and 3 = α-lactalbumin and BSA. A 3000SW plus 2000SW column system with a 30 μl injection volume yielded four protein peaks: 1 = minor amounts of α - and β-casein; 2 = casein, BSA and IgG; 3 = β-lactoglobulins; and 4 = α¹-lactalbumin. A 3000SW plus 2000SW column system with a 10 μl injection volume yielded five protein peaks: 1 = casein; 2 = IgG; 3 = BSA; 4 = β-lactoglobulins; and 5 = α-lactalbumin. Both the single column and dual column applications yielded three nonprotein peaks, which were dialyzed from solution. Thus, a high speed analytical separation of milk proteins was achieved according to molecular size, but this application is highly dependent on sample size.     

Protein-calixarene interactions: complexation of Bovine Serum Albumin by sulfonatocalix[n]arenes

The complexation of Bovine Serum Albumin with sulfonatocalix[n]arenes has been demonstrated by means of electrospray mass spectrometry, dynamic light scattering and atomic force microscopy; with sulfonatocalix[4]arene one strong and two weaker binding sites are detected; the effects on the structure of thin films formed by surface deposition of BSA show that the sulfonatocalix[n]arenes act to reticulate the films and produce essentially planar systems.     

Determination of antimony,arsenic, bismuth and copper by inductively coupled plasma atomic emission spectrometry in the electrorefining of copper

Inductively coupled plasma atomic emissionspectrometry (ICP-AES) has been applied as a rapid and routine method for the analysis of process electrolytes in the electrorefining of copper. Antimony, arsenic, bismuth and copper have been selected as major electrolyte constituents. For these elements profound statistical studies of spectral and interelement effects have been carried out. For As, Bi and Sb two analyte wavelengths have been selected, and for Cu one relatively insensitive analyte line has been chosen due to the high Cu concentration in samples. Best analytical lines were: As at 193.759 nm, Bi at 306.772 nm, Sb at 206.833 nm and Cu at 216.953 nm. Multiple linear regression proved to be very capable in the search of the best analytical wavelength and identifying interfering elements. Using simple acid based standards all elements investigated can be determined separately in complicated matrices with satisfactory results. Differences between true values and measured values can be partly eliminated by appropriate calculational methods.     

Determination of trace elements in various organs of rats by thermal neutron activation analysis

The trace element levels in various organs of normal rats have been determined by means of thermal neutron activation followed by high-resolution gamma-spectroscopy. Abundances for 11 elements (Cu, Mn, Fe, Zn, Rb, Sb, Se, Cr, Co, Cs and Sc) were evaluated in the individual subjects. The present results were generally found within the ranges of the literature values, except for ultra-trace elements. Reliability of the method was assessed by analyzing NBS standard reference materials, Orchard Leaves and Bovine Liver. The trace element contents of the rat diet have also been measured, and comparison of them with those of the rat organs was given.     

Graft Copolymerization of 2-Hydroxyethyl Methacrylate onto Bovine Serum Albumin: Preparation and Characterization

ABSTRACT

Bovine Serum Albumin (BSA) was separated from the whole blood of freshly slaughtered animals. This BSA was graft copo-lymerized with poly (2-hydroxyethyl methacrylate) and characterized. The infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and percentage of grafting of the composites were studied. The graft copolymers have better physico-chemical properties and, therefore, could be more useful in their field of application.     

Hydrogeological application of trace element analysis with ICP-AES for the characterization of groundwater categories at the foot of the Swiss Jura between Geneva and Lausanne

Summary Different groundwater categories have been recognized at the foot of the Jura mountains between Geneva and Lausanne. This categorization relates to the geological nature of the aquifer as well as the flow system to which the studied groundwaters belong. Further characterization based on the hydrochemical content of the water has been attempted. Special attention has been paid to the trace elements. Due to the very low detection limits of the ICP-AES, the accuracy of the analyses and the good reproducibility of the measurements, some trace elements have proven to be of interest for characterizing groundwaters (alimentation, aquifer, flow system). The paper describes results of a combined interpretation of barium concentration and electrical conductivity in groundwaters, as well as the trace analytical conditions which made an accurate determination of the trace elements possible. It shows that trace elements can contribute to a better understanding and protection of groundwaters.     

Studies on Permeation of Bovine Serum Albumin (BSA) Through Photo-Modified Functionalized Asymmetric Membrane

UV-initiated photo-modification by hydrophilic functional moieties (viz. acrylic acid, acrylamide) is performed on the photo-responsive Polyether sulfone (PES) membrane. Characterization of the modified membranes has been done by porometry, Fourier Transform-IR (FTIR), contact angle, thermogravimetry, X-ray diffraction and gel permeation chromatography. The grafting of acrylamide is higher compared to acrylic acid, as is evidenced from weight increase, as well as porometry studies. The separation abilities of Bovine Serum Albumin (BSA) have been experimented through all the membranes and results show that modified membranes possess a better separation ability compared to virgin polyether sulfone. The separation order follows the trend: PES-g-(AM) > PES-g-(AA) > PES. pH dependence conformational changes of BSA macromolecule influence the separation. The increase in pH results in the decreasing trend in separation. The water flux recovery ratio (FRR) for the virgin PES membrane is minimum compared to other two grafted membranes.