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PubMed1995

Chromium speciation by anion-exchange high-performance liquid chromatography with both inductively coupled plasma atomic emission spectroscopic and inductively coupled plasma mass spectrometric detection.

Development of a new method for the determination of Cr(III) and Cr(VI) is described. Anion-exchange high-performance liquid chromatography (HPLC) was used to separate Cr(III) and Cr(VI) with on-line detection by inductively coupled plasma atomic emission spectroscopy (ICP-AES) at 2766 A in preliminary studies, and inductively coupled plasma mass spectrometry (ICP-MS) with single-ion monitoring at m/z 52 and m/z 53 for final work. A mobile phase consisting of ammonium sulfate and ammonium hydroxide was used, and a simple chelation procedure with EDTA was followed to stabilize the Cr(III) species in standard solutions. ICP-MS results indicated the feasibility of using chromium isotope m/z 53 instead of the more abundant m/z 52 isotope due to a high mobile-phase background most significantly from the SO+ polyatomic interference. The absolute detection limits based on peak-height calculations were 40 pg for Cr(III) and 100 pg for Cr(VI) in aqueous media by HPLC-ICP-MS. The linear dynamic range extended from 5 ppb (ng/ml) to 1 ppm (micrograms/ml) for both species. By HPLC-ICP-AES, detection limits were 100 ng for Cr(III) and 200 ng for Cr(VI). Cr(III) was detected in NIST-SRM 1643c (National Institute of Standards and Technology-Standard Reference Material, Trace Elements in Water) by HPLC-ICP-MS at the 20 ppb level.

Chromatography, High Pressure Liquid↗
PubMed1994

A method for the determination of environmental contaminants in living marine mammals using microscale samples of blubber and blood.

As part of a study examining the possible effects of organochlorine compounds on juvenile northern elephant seals (Mirounga angustirostris), blubber and blood samples were taken from animals present on the Año Nuevo (California) rookery, and from animals admitted for rehabilitation at The Marine Mammal Center (Sausalito CA). Blubber samples were collected from immobilized seals. A pre-cleaned 6 mm K-medic biopsy punch was used to extract the blubber from a 1 cm incision near the hip, near the dorsal mid point. Blood samples were taken from the extradural vein; two mL of serum was analyzed for organochlorine compounds. Blubber samples (approximately 0.1g) were ground with Na2SO4 and extracted with 20 mL hexane:methylene chloride (1:1). Sera samples were extracted using commercially available disposable C18 columns. The extracts were separated on a micro-Florisil column, and analyzed by HRGC-ECD. Lipid determination in the serum was obtained by colorimetric analysis with 20 microliters samples. Results from the analysis of replicates and standard reference materials showed good recoveries, precision, and accuracy for both the blubber and blood methods.

Adipose Tissue↗
PubMed1996

Interlaboratory comparison study for PCB congeners and chlorinated pesticides in beluga whale blubber.

Three laboratories participated in an interlaboratory comparison exercise for the determination of polychlorinated biphenyl (PCB) congeners and chlorinated pesticides in Standard Reference Material (SRM) 1588 (Organics in Cod Liver Oil) a whale blubber control material, and six beluga whale (Delphinapterus leucas) blubber samples. The results are generally in good agreement. The minor disagreement of some of the results may be attributed to differences in detector calibrations, differences in chromatographic separation selectivity for specific compounds, or both. The SRM and control material help to validate the analytical procedures and to verify that these procedures remain in control.

Adipose Tissue↗
PubMed1992

Trace quantitation of 4-hydroxy-2-nonenal in biological samples as its oxime-bis-tert.-butyldimethylsilyl derivative using 3-hydroxynonanal as an internal standard.

A gas chromatographic-mass spectrometric method for the determination of the lipid aldehyde 4-hydroxy-2-nonenal (4HNE) in trace quantities is described. The method utilizes the reaction of aldehydes with hydroxylamine leading to the formation of the oxime derivative. The aldehydes are recovered by octadecylsilyl solid-phase extraction and converted to the bis-tert.-butyldimethylsilyl derivatives for analysis using electron ionization. A novel 4HNE analogue, 3-hydroxynonanal, has been synthesized and is used as an internal standard. A limit of detection of approximately 1 pmol of 4 HNE in preparations of approximately 2.10(6) cells or 0.5 ml of whole blood, plasma or serum was observed. Standard addition analysis indicates that the method is accurate at these levels. Replicate analysis of the National Institutes of Standards and Technology Standard Reference Material SRM 909 indicates an average in-run precision of 8.1% and a between-run precision of 13.5% at an average concentration of 82.1 pmol/ml of reconstituted material.

Aldehydes↗
PubMedDate not supplied

An evaluation of the environmental implications of petroleum refinery emissions by multielemental neutron activation analysis of rumen fluid ash of buffaloes.

In order to study environmental pollution in and around a petroleum refinery complex, a multielemental instrumental neutron activation analysis (INAA) method was used to assay concentrations of As, Ba, Br, Cl, Co, Cr, Cs, Cu, Fe, Hg, La, Mn, Mo, K, Na, P, Sc, Rb, Se, Sr, W and Zn in the rumen fluid ash samples of buffaloes from the vicinity of the refinery. Corresponding samples from a control area 300 km away from the refinery were analysed. Standard Reference Materials, Bovine liver (SRM 1577a), Oyster tissue (SRM 1566a) and Animal bone (CRM H-5) were also analysed for quality control. Samples were irradiated with thermal neutrons at 10(12)-10(13) n cm-2 s-1 and counted by high-resolution gamma spectrometry. Mean elemental concentrations of As, Ba, Br, Cr, Hg and Fe were found to be enhanced, whereas those of Na, K, Cl, Cu, Mn and P were depleted in samples from the vicinity of the refinery complex compared to controls. The environmental implications of anomalous elemental concentrations are discussed.

Animals↗
PubMed2004

Data evaluation of trace elements determined in Nigerian coal using cluster procedures.

Large data-sets of elements determined by instrumental neutron activation analysis (INAA) require meaningful interpretation in order to determine the pattern of their existence in host matrices. This could be achieved using cluster procedures. Element abundances (Al, As, Ba, Br, Ca, Ce, Cs, Dy, Eu, Fe, Ga, Gd, Hf, K, La, Lu, Mg, Mn, Na, O, Rb, Sb, Sc, Sm, Sr, Ta, Tb, Th, Ti, U, V, Yb, Zn and Zr) of prepared and run-of-mine coals from eight principal mines (Onyeama, Ogbete, Enugu, Gombe, Asaba-Ugwashi, Okaba, Afikpo and Lafia ) in Nigeria were determined by INAA. Quality control of the measurements was assured by the re-determination of a standard reference material, NIST 1632a. These data-sets were then tested for multi-variate statistics using METHOD = SINGLE in the cluster procedure. The computer-assisted package SAS was used to generate the dendrograms while the algorithm used was stored Euclidean distances. The results showed a recognition pattern, useful for the interpretation of coalification histories and the prediction of fuel ranking for Nigerian coals. High segregation of coal fly ash was observed, while metallurgical coal grouped together with high-ranking coals of Okaba, Enugu and Obi (Lafia). Further work revealed some of these coals as having high gross calorific value (7908 kcal kg(-1) for Enugu coal; 7200 kcal kg(-1) for Okaba) and low sulphur thereby making them efficient fuel materials.

Cluster Analysis↗
PubMed2004

Development and application of Marinelli beaker standards for monitoring radioactivity in Dairy-Products by gamma-ray spectrometry.

Marinelli (reentrant) beakers are recommended for measurement of low-activity radioactive environmental samples, in both liquid and solid phase. The preparation of Marinelli beaker standards of milk powder containing 232ThO2 at secular equilibrium with its daughter radionuclides was studied. Standards were prepared by mixing of known amounts of solid ThO2 and milk powder. The densities of the standards were 0.5-0.7 kg dm(-3). Measurements of calibrated Marinelli beaker standards with HPGe detector showed that the energy dependence of the efficiency is similar to that of a point source, i.e. an almost linear dependence of log-efficiency vs. log-energy in the 200-2000 keV range, however the parabolic correlation fits better. The validity of these standards was checked by comparison with certified standard reference material IAEA-152-Milk powder containing radiocesium and radiopotassium. The results obtained were found to be in a good agreement with the published certified data. The limit of detection for the determination of radiocesium by gamma ray spectrometry under the prevailing experimental conditions is 0.03 Bq (i.e. 0.8 pCi), for samples of dairy products having lower densities of 0.7 kg dm(-1).

Dairy Products↗
PubMed2006

Qualification and performance characteristics of a quantitative enzyme-linked immunosorbent assay for human lgG antibodies to anthrax lethal factor antigen.

The contribution of Bacillus anthracis lethal factor (LF)-specific immune responses to protection against anthrax disease in humans remains incompletely defined due, in part, to a paucity of qualified reagents and a lack of standardized serological assays. Toward this end, we have identified and characterized suitable positive quality control and standard reference sera and developed, optimized, and qualified an enzyme-linked immunosorbent assay (ELISA) to measure LF-binding IgG. Herein we describe the performance characteristics of this ELISA and propose criteria for its use in the detection and quantification of anti-LF IgG in human serum.

Anthrax↗
PubMed2005

Microscale analytical methods for the quantitative detection of PCBs and PAHs in small tissue masses.

Microscale methods (MM) were evaluated and compared to traditional methods (TM) for measuring polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) in spiked and standard reference fish and mussel tissues. MMs are advantageous because they use small tissue masses (ca. 100mg), and maintain sensitivity through reducing final extract volume (traditionally 1 ml) by an order of magnitude or more (40 microl-PCBs; 100 microl-PAHs). Procedural losses occurred in the MMs' combined cleanup/primary evaporation step (19% PAHs; 6% PCBs), and the final extract concentration (14% PAHs; 22% PCBs). The PAH MM performed comparably to the TM. Although most PCBs had recoveries >50%, the PCB MM generally yielded lower recoveries than the TM. Average method detection limits were 0.6 microg/kg (TM) and 1.0 microg/kg (MM) for PCBs and 25.7 microg/kg (TM) and 27.7 microg/kg (MM) for PAHs. MMs described for PCB and PAH tissue samples are potentially viable alternatives to TMs, and could lead to cost savings in bioaccumulation/toxicity tests.

Animals↗
PubMed2005

Spectrophotometric determination of uranium with arsenazo-III in perchloric acid.

A short, sensitive and reliable spectrophotometric method, which has advantages over all known "wet chemistry" methods for uranium determination with regard to tolerance to common interferences, has been developed for the determination of uranium. Selectivity, molar absorptivity and the determination range of uranium have been enhanced by using 0.07% arsenazo-III as a chromogenic reagent. The use of 3 mol dm(-3) perchloric acid as a medium of determination was found to be excellent in terms of good solvent compatibility on dilution, destruction of organic contamination and simplicity of operation. The uranium-arsenazo-III complex formed instantly, and was found to be stable for more than 3 weeks with constant absorbance. Beer's law was obeyed up to a uranium concentration of 16 microg g(-1), with a molar absorptivity at 651 nm of 1.45x10(5) mol(-1) dm(3) cm(-1) at 24+/-2 degrees C. Only phosphate and citrate at 70-fold excess over uranium interfere seriously, whereas other anions studied could be tolerated up to a 70-fold excess over uranium. Of the cations studied, only Mn(II), Co(II), Ni(II), Cu(II) and Cr(III) decreased the normal absorbance of the complex. Iron(III), Ce(III) and Y(III) enhanced the absorbance. Other cations studied did not affect the absorbance up to a 50-fold excess. The accuracy was checked by determining uranium from standard solutions in the range 10-50 microg g(-1). It was found to be accurate with a 96.0-98.6% recovery rate. The method has been successfully applied to standard reference materials and ore samples at microg g(-1) levels.

Absorption↗
PubMed2006

Improved chromatographic separation of thio-arsenic compounds by reversed-phase high performance liquid chromatography-inductively coupled plasma mass spectrometry.

A new group of arsenic species, thio-arsenicals, have recently been reported in several natural samples such as molluscs, algae, and urine. These compounds are the sulfur analogues of oxo-arsenicals, a large group of naturally-occurring compounds, whereby the arsinoyl (As=O) group is substituted by an arsinothioyl group (As=S). The most common separation technique for oxo-arsenicals is anion-exchange HPLC with polymer-based columns, but under these conditions the thio-arsenicals show strong retention, resulting in unacceptably long analysis times and broad peaks. We report the development of a reversed-phase HPLC method, with ICPMS detection, which allows separation of the known thio-arsenicals within 15 min with significantly improved peak shapes. The detection limit is about 0.6 microg As/L based on 10 microL injection volume. Further, we have applied the method to the identification and quantification of thio-arsenic species in two standard reference materials, BCR 710 oyster tissue and NIES 18 human urine.

Animals↗
PubMed2004

Microanalysis of non-heme iron in animal tissues.

The method recommended by the Iron Panel of the International Committee for the Standardization in Haematology for measurement of serum iron was adapted for measurement of non-heme iron in animal tissues. The method developed was designed specifically to facilitate measurement of non-heme iron using as little as 10 mg of tissue, in a final reaction volume of 60 microl. In this assay, tissue homogenates are treated with hydrochloric acid and trichloroacetic acid and heated at 95 degrees C. Non-heme iron is released and protein is precipitated. Following centrifugation, iron in the supernatant is reacted with ferrozine in the presence of the reducing agent thioglycolic acid, and the complex is quantified by spectrophotometry. The method was validated by analysis of two Standard Reference Materials (bovine liver), comparing results of this assay against certified values and concentrations determined by flame atomic absorption spectrometry following acid digestion. Results using this method for analysis of non-heme iron in guinea pig tissues (liver, kidney and heart) compared favorably with those obtained using micro-scale adaptations of three published reference methods. The new method was more sensitive, required less time, and was less cumbersome than the three published methods to which it was compared.

Animals↗
PubMed2006

Celtek clay as sorbent for separation-preconcentration of metal ions from environmental samples.

The sorption conditions including pH of the aqueous solution, sample volume, etc., on Celtek clay of copper(II), cadmium(II), lead(II), chromium(III), nickel(II) and cobalt(II) ions from environmental samples has been studied. The effects of electrolytes as matrix on the preconcentration were also investigated with the recoveries >95%. The 3 sigma detection limits for copper, cadmium, lead, chromium, nickel and cobalt ions were found to be 0.25, 0.32, 0.73, 0.45, 0.50 and 0.41 microg/l, respectively. The relative standard deviation was <10% for the determination of analytes. The procedure was validated by analysis of a NRCC-SLRS 4 Riverine Water, SRM 1573a Tomato leaves and IAEA 336 Lichen standard reference materials. The developed method was successively utilized for the determination of Cu(II), Cd(II), Pb(II), Cr(III), Ni(II) and Co(II) in various samples including natural waters, wheat and human hair by flame atomic absorption spectrometry (FAAS) with satisfactorily results (recoveries>95% and R.S.D.'s<10%).

Adsorption↗
PubMed2006

On-line arsenic co-precipitation on ethyl vinyl acetate turning-packed mini-column followed by hydride generation-ICP OES determination.

An alternative and new system for on-line preconcentration of arsenic by sorption on a mini-column associated to hydride generation--inductively coupled plasma--optical emission spectrometry determination was studied. It is based on the sorption of arsenic on a column packed with ethyl vinyl acetate (EVA) turnings and the use of La(III) as co-precipitant reagent. This polymeric material was employed here for the first time as filling material for column preconcentration. It could work both as adsorbent and as sieve material. Sample and co-precipitant agent (lanthanum nitrate) were off-line mixed and merged with ammonium buffer solution (pH 10.0), which promoted precipitation and quantitative collection on the small EVA turnings. The arsenic preconcentrated by co-precipitation with lanthanum hydroxide precipitate was subsequently eluted with hydrochloric acid, which was the medium used for hydride generation. Considering a flow rate of 5 ml/min, three enrichment factors were obtained, 28-, 38- and 45-fold at three different sampling times, 60, 120 and 180s; respectively. The detection limits (3s) obtained for each case were 0.013, 0.009 and 0.007 microg/l. Additionally, the calculated precisions expressed as relatively standard deviation (R.S.D.) were 0.9, 1.3 and 1.1%. Satisfactory results were obtained for the determination of arsenic in standard reference material NIST 1643e Trace Elements in Water and drinking water samples.

Arsenic↗
PubMed1999

Determination of niobium(V) and tantalum(V) as 4-(2-pyridylazo)resorcinol-citrate ternary complexes in geological materials by ion-interaction reversed-phase high-performance liquid chromatography.

A method for the simultaneous separation and determination of Nb(V) and Ta(V) as ternary complexes formed with 4-(2-pyridylazo)resorcinol (PAR) and citrate was developed using ion-interaction reversed-phase high-performance liquid chromatography on a C18 column. Method parameters, such as pre-column complex formation conditions and composition of the complexes were investigated using spectrophotometry and HPLC. Under the optimum conditions, the Nb(V) and Ta(V) complexes were eluted within 12 min with a mobile phase of methanol-water (32:68, v/v) containing 5 mM acetate, 5 mM TBABr and 5 mM citrate buffer at pH 6.5, with detection at 540 nm. A typical separation efficiency was 33,000 and 20,000 theoretical plates per metre for Nb(V) and Ta(V), respectively. The relative standard deviation of retention times for the Nb(V) and Ta(V) complexes were 0.16% and 0.17% and for peak areas were 0.28% and 1.36%, respectively. The detection limits (signal-to-noise ratio = 3) for Nb(V) and Ta(V) were 0.4 ppb and 1.4 ppb, respectively. Results obtained for standard reference rock samples agreed well with certified values and results obtained by inductively coupled plasma MS.

Chromatography, High Pressure Liquid↗
PubMed1984

The aluminum content of biological products containing aluminum adjuvants: determination by atomic absorption spectrometry.

Aluminum compounds are used as adjuvants in certain types of vaccines, toxoids and allergenic extracts for human use. The most common Al compounds used in biological products to enhance the immune response are aluminum potassium sulphate (alum), aluminum hydroxide and aluminum phosphate. This study describes an atomic absorption spectrometric method for the determination of the Al content of Al adsorbed toxoid preparations and allergenic extracts at levels of less than 0.85 mg of Al per half millilitre human dose. Aliquots of the samples which contained Al suspensions were acid digested with nitric and sulphuric acid and analysed in the nitrous oxide-acetylene flame of an atomic absorption spectrometer. The 396.2 nm Al line was used for analysis. The Al content of the National Bureau of Standards (NBS) Standard Reference Material No. 1075a aluminum 2- ethylhexanoate was determined to within 1% of the NBS certificate value by this method. Atomic absorption results for the Al content of tetanus toxoids containing aluminum potassium sulphate and aluminum phosphate were compared with polarographic and inductively coupled argon plasma (ICP) emission spectrometry results. Reproducibility and recovery data for Al are tabulated for a variety of biological products containing aluminum phosphate, aluminum potassium sulphate and aluminum hydroxide adjuvants. In addition, ICP has been used to characterize the Al and P compositions of the precipitates and supernatant solutions which resulted from centrifuging toxoid suspensions that contained the three different Al adjuvants.

Adjuvants, Immunologic↗
PubMed2003

Determination of zinc, copper, lead and cadmium in some medicinally important leaves by differential pulse anodic stripping analysis.

Levels of zinc, copper, lead and cadmium have been determined in some medicinally important leaves by differential pulse anodic stripping voltammetry (DPASV). High pressure digestion with nitric acid (HPA) was used for sample digestion. The accuracy of the method was verified by the parallel analysis of leaves with inductively coupled plasma atomic emission spectroscopy (ICP-AES) and recovery studies by the analysis of standard reference materials. Based on elemental levels the utility of these leaves in medicine are discussed. Statistical treatment has been used in order to understand the correlation between elements in these leaves.

Animals↗
PubMedDate not supplied

Measurement of 90Sr in bone ash.

Bone is a critical organ for the accumulation of many radionuclides, including 90Sr. A bone ash has been prepared by NIST to become a standard reference material and the assaying of the 90Sr activity concentration is reported. A radiochemical procedure, based on extraction chromatography using a crown ether, has been developed to separate Sr from the bone ash. The natural Sr content of the bone ash has been determined by isotope dilution inductively coupled plasma mass spectrometry. The 90Sr activity concentration has been measured by low-level liquid scintillation counting.

Animals↗