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L Ebdon

Publications and source records attributed to L Ebdon.

10 recordsLinked to original sources

Trends in certified reference materials for the speciation of trace elements.

The measurement of the chemical species of elements (instead of the total element concentration) has become an irreversible trend in analytical chemistry. The motivation lies in the fact that the biochemical and geochemical behaviour of an element is governed by its species. Quality assurance of the analytical procedures used for speciation analysis requires the analysis of representative reference materials, certified for the relevant species. Up to now the number of existing certified reference materials for trace element species is very limited. The most important ones are environmental CRMs certified for trialkyltin compounds, methylmercury, Cr(III)/Cr(VI) and food CRMs certified for arsenic species and methylmercury. Major developments are to be expected in CRMs focussed on environmental problems, including waste treatment, on bioavailability of trace elements in food and on bio-monitoring in occupational health and hygiene. It is, however, unlikely that the producers of CRMs will ever be able to cover all needs. Add to this that many, very active species are notoriously unstable and/or short living and require in-situ analysis. This will lead to different analytical developments, such as analyses in-situ, where the classical concept of CRMs may not stand firm anymore.

Animals↗

Partitioning of mercury onto suspended sediments in estuaries.

Radiochemical partitioning experiments using 203Hg have been undertaken with mixtures of river, seawater and sediment samples taken from three geochemically contrasting UK estuaries: the Plym, Beaulieu and Mersey. Species of dissolved Hg were determined using reversed-phase C18 chelating columns and particulate species were determined by sequential leaching with 1 M NH4OAc and 1 M HCl. Mercury had a high particle reactivity with partition coefficients, KDs, ranging from 10(4) to 5 x 10(5) ml g(-1), depending on salinity, the chemical composition of the end-member waters, and on the physico-chemical characteristics of the sediment. Dissolved organic matter present in the waters (humic substances and/or anthropogenic compounds) was found to be the main factor governing the forms of dissolved Hg and their reactivity. From the spiked 203Hg, up to 95% of the dissolved metal was retained on the C18 columns for the Mersey waters, whereas this fraction was < 60% in the Plym and Beaulieu waters. Quasi-irreversible adsorption of Hg onto particles from each estuary was observed over a time-scale of a few hours and < 20% of total particulate Hg was released by the sequential leach. In this paper, physico-chemical processes are proposed to explain the estuarine behaviour of Hg and the results are discussed in terms of Hg availability in estuarine systems.

Adsorption↗

A preliminary clinical investigation into the potential of blood lead levels to measure bone resorption in patients with skeletal metastases, using ICP-MS.

A simple, accurate and precise method to measure lead levels in whole blood by inductively coupled plasma-mass spectrometry (ICP-MS) has been developed. Blood samples were diluted (1 + 9) with 0.1% v/v Triton X-100 and 0.1% v/v nitric acid, and gave a limit of detection of 0.06 microgram/l (3sn). Spiking experiments demonstrated recoveries of 100 +/- 10% and verification against Seronorm reference and BCR certified reference materials gave experimental values in close agreement to the reference values. The methodology was used to conduct a feasibility study, involving a preliminary clinical investigation to assess the potential of whole blood lead levels as biochemical markers to measure bone resorption in patients with skeletal metastases and receiving treatment. The results from this feasibility study showed that the method remained under analytical control, giving inter and intra assay coefficients of variation of < 5%. This feasibility study also showed that the changes in the blood lead levels within individual patients were measurable and in many cases the patient's observed clinical performance demonstrated similar trends to the blood lead levels measured over time. Overall the results were encouraging and showed promise. Further and more detailed investigations into the use of lead and other trace metals as biomarkers of bone resorption is warranted.

Aged↗

A high performance liquid chromatography - inductively coupled plasma-mass spectrometry interface employing desolvation for speciation studies of platinum in chemotherapy drugs.

A novel interface between high performance liquid chromatography (HPLC) and inductively coupled plasma-mass spectrometry (ICP-MS) is described. The eluent from the HPLC is nebulised into a heated cyclone spray-chamber and the solvent removed using a Nafion membrane drier, held at 75 degrees C, and a cryogenic condenser. The condenser consists of 6 Peltier heat pumps connected to liquid cooled aluminium blocks. At a nebuliser gas flow rate of 0.6 l min(-1), the membrane drier removes 58% of the vapour and the Peltier condenser 75% of the remaining vapour, i.e. a total desolvation efficiency of 89%. This enables the use of HPLC solvents which otherwise would destabilise the ICP, e.g. 100% acetonitrile or methanol, and permits the use of solvent gradients with minimal baseline drift. The system has been applied to the determination of platinum species in an organoplatinum drug used for chemotherapy in human plasma ultrafiltrate of patients treated with this new drug (JM-216). The limit of detection for platinum species has been 0.6 ng nl(-1) (i.e. 120 pg of Pt) and several species have been separated with good resolution.

Journal Article↗

The accumulation of organotins in adult and seed oysters from selected estuaries prior to the introduction of U.K. regulations governing the use of tributyltin-based antifouling paints.

Between April and November, 1985, a study of the levels of organotins in adult and seed Crassostrea gigas grown in the southwest and southeast of England was carried out. This work corresponds with a similar study of organotin water levels (reported separately). The analytical procedure used was directly coupled high performance liquid chromatography-flame atomic absorption spectrometry. Individual adult oysters and groups of 20-40 seed oysters were taken for analysis on a monthly basis. The profiles of tributyltin (TBT), dibutyltin (DBT) and monobutyltin (MBT) are discussed in relation to each other and levels found in the waters. In general, levels of all three organotin species were found to be higher in the seed oysters. Mean levels of TBT reached 3.1 micrograms g-1 in seed oysters from the Exe, Devon, in October, whereas mean levels of DBT and MBT reached 16.1 and 16.7 micrograms g-1 in Teign, Devon, seed oysters in October. Bioconcentration factors of approximately 1000 were found, but seem to be greater when lower levels of TBT were present in the water, perhaps indicating a more 'efficient' removal from the water. The degree of shell thickening was calculated for all oysters submitted for analysis. The highest percentage of adult oysters with severely thickened shells was found at Tollesbury Fleet, where 61% of oysters showed shell thickness index values of six or less. Generally, two peaks in TBT levels in the oysters were observed, in the late spring and early summer: these seem to correlate with peak levels of TBT in the waters immediately preceding these times. A large proportion of the DBT and MBT found in the oysters seems to come from the metabolism of the TBT ingested. It is suggested that high sediment loadings may contribute to the severe deformation of oysters grown at Tollesbury Fleet, but only in the presence of TBT.

Aging↗

Application of high-performance liquid chromatography--inductively coupled plasma mass spectrometry to the investigation of cadmium speciation in pig kidney following cooking and in vitro gastro-intestinal digestion.

The speciation of cadmium in retail pig kidney has been examined by size-exclusion chromatography (SEC) coupled directly to inductively coupled plasma mass spectrometry (ICP-MS). Approximately 35% of the cadmium from uncooked kidney was soluble after aqueous extraction at pH 8 and SEC - ICP-MS revealed three discrete peaks whose retention times corresponded to estimated relative molecular masses of 1.2 x 10(6), 7.0 x 10(4) and 6 x 10(3)-9 x 10(3). In the cooked kidney, 35% of the Cd was soluble and was all associated with a peak of a relative molecular mass (Mr) of 6 x 10(3)-9 x 10(3). After simulated gastric digestion of cooked pig kidney at pH 2.5, 60% of the cadmium was solubilised and associated with a species of Mr less than 1 x 10(3). When the digest was also subjected to simulated intestinal digestion at pH 6.8, a single peak, which corresponded to 20% of the original cadmium, was eluted. This peak co-eluted with the single peak extracted at pH 8.0 from the cooked kidney. It was also of similar estimated Mr to the single broad peak observed after simulated gastro-intestinal digestion of equine renal metallothionein (Mr = 1.1 x 10(4]. The results suggest that the majority of soluble cadmium in retail pig kidney is associated with a metallothionein-like protein that survives both cooking and simulated in vitro gastro-intestinal digestion.

Animals↗

Isotope ratio and isotope dilution analysis of lead in wine by inductively coupled plasma-mass spectrometry.

The lead content of 12 wine samples was measured by inductively coupled plasma-mass spectrometry using the methods of standard addition and isotopic dilution analysis. An additional wine sample was analysed by external calibration, standard addition and isotopic dilution analysis. The lead content of the wine samples was in the range 30-150 ng ml-1 and good agreement between the different techniques was observed. Analysis of lead isotope ratios revealed significant differences between Australian and European wines, reflecting the different isotopic composition of Australian lead.

Australia↗